Document po1Qg87p2kEpoMNRbO66enjj

INTER-OFFICE CORRESPONDENCE To: 3. R. Hopper H. K. Kaster 3. F. Knight P. Fiedler Hooker Chemical Company Date: From: Subject: March 30, 1981 3. 6. Parsons Shell Toll Fee RECEIVED APS 11981 ** R. HOPPER Effective April 1, 1981, and until further notice, the toll fee for VCM from Shell will be 15.5^/pound. This equates to a chlorine value, including pipeline charges, of $78/ton. JGP/akf 0429m V C )rf/K 1 Parsons 4-3-9 f OXY/HOLMES 001103 n n BUCO owwM '.cH D. A. Bloomfield Copies toi B. Harrison w. Howells H. Kastex A. Katona J. Ruffing M. Soble A. Tybus P. Weill W. Wetzel r~ f Subject: SPI AD HOC VCM/PVC MEETING INTER-OFFICE MEMORANDUM File Hf,: RJA; 293-74M Date: April 17, 1974 From: R, J. Abramowitz Div./Dep't: RUCO/Polymers Location: Burlington ABSTRACT A meeting of the special SPI Ad Hoc VCM/PVC Group was held in Washington, D. C. on April 16th, 1974 for the purpose of organizing a coordinated industry response to , the recent OSHA "Emergency Temporary Standard For Exposure to Vinyl Chloride." A copy of the agenda is attached. There were approximately 50 attendees. Monitoring of VCM in plant areas and in polymers is being conducted vigorously in all plants. The feeling was that OSHA is moving towards a permanent standard of zero exposure, with a possible imminent revision of the temporary standard to a level some what below 50 ppm of VCM in work areas. A committee was appointed to formulate a response to OSHA which will stress: 1. The satisfactory human experience in properly regulated VCM/PVC plants in operation for more than 20 years. 2. Time required by industry to conform to new OSHA regulations. 3. Support of additional animal exposure test at levels below 50 ppm of VCM. 4. Need for accurate definition of test methods, test equipment, protec tive devices, etc. 5. An economic impact statement regarding effect on the country of zero production. Tne group unanimously agreed that the entire industry would shut down if the regulations called for a maximum VCM exposure of ippm. Two or three producers thought they could live with 30 ppm (TWA), if absolutely necessary, while a majority agreed that they would find a way to cope with a level of 40-50 ppm. It was agreed that more VO! data is required in PVC processing areas and this will be accumulated. CBS is planning a one hour TV Documentary on the Vinyl Chlqride-PVC problem. Industry was urged not to obstruct this effort for PR purposes. RJA/kr ofm ho. ft. J, Abramowitz OCC 1561 t Li * gflaoker RUCQ 9MtWH Tm Copies tot R. J. Abramowit2 C. W. Corbin L. J. Friedman B. P. Hirsch W. D, Howells H. H. Kaster Tybus**?#.. 11/ u Subject; GC RECENT ARTICLES :r-office memorandum FittRet; RVL:398-73M Date-. June 20, 1973 Froms R. V. Lucke Div./D*p*fe RUCO/Polymers Location: Burlington Attached are several recent articles ran GC utilization. Pages 74 and 42 have reasonable summaries for general review. I thought you might be interested in view of our heavy recent involvement in VCM quality and the FDA problem. RVL/cac OCC 1716 H \ \X i *! H I! J* i Herbert L Kobe end Zone BitterlMd TerkhhEhner Corp. 1-R UP-DATE HPLC (Liquid Chromatography) state of rheart 1973 Tim ANALYTICal TEcmttQOE of dmmatography is, by any standard, one of the die sample is separated into its components, which emerge from the'end of the column at most powerful that has ever been developed*different times, and pass through a suitable Almost every analytical laboratory--and cer detector. tainly my laboratory that is concerned with Liquid column chromatography has been the analysis of organic materials (including, understood m principle for at least 50 years, of course, those in the life sciences)--is but until recently suitable equipment, equipped with some farm of chromatographic particularly pumps and detectors, has not instrumentation. It may be a gas chromato been available. graph or die equipment to perform thin layer A typical liquid chromatographic column is or paper chromatography. 500 sun long, has an inside diameter of about And now increasing interest is being shown 2 mm, and is packed with spheres 10 to 30 in ltqmd column chromatography, also known microns in diameter* Unless high-pressure as high pressure liquid chromatography pumps are employed, the elution of a sample (HPIX2). Ibis was known formerly as liquid from such a column would take many hours chromatography, bid: researchers prefer a or even days* more-precise tern since other techniques also Now, however, it is common to use pump involve liquid m the process* pressures of 1,000 to 3,000 psi (70 to 220 HPLC, die major subject of this article, has kg/cm*) and constant-flow pumps capable of the curious distinction of being at once the 7,000 psi (500 kg/cnv1) have recently been oldest and die newest of the chromatographic introduced. With such pomps, an analysis techniques. In its simplest form, HPLC can be can be completed in several minutes. regarded as an increase in the sophistication A typical sample site for a high pressure of paper atul thin layer techniques* liquid chromatograph is 10 to 20 /J, while sol The sample is injected into a chromato vent flow rates are of the order of 0.5 to 5 ml graphic column through which a suitable per minutc. It requires only a simple c<mimpu solvent is being pumped* In&klc die column. tation to lead to the conclusion that the diin- OCC 1717 RSAC*WU* tm tion of the sample is very great, placing great demand-, on thv* detector located at the end of the eluomatugraphic column. At present two types of detectors, RJ and Uth arc in general use. The refractive index detector measures differences in the optical refractive index, comparing the refractive index of the pure solvent to that of solvent plus sample. The output of the detector appears as a recorder peak where the area depends on the concentration of the sample component being measured, ax well as on the difference between the refractive indices of the solvent mid die sample component Until recently, refractive index detectors had mystifying problems and irritating in stabilities. Now, however, detectors are available which can reliably measure differ ences of 10-8 units in refractive index. (As a standard of comparison, the refractive index of a vacuum is defined as 1.0, while that of ordinary window glass is approximately 1.5.) Most materials have the ability to absorb radiation at ultraviolet wavelengths- Therefore an alternative detector, which frequently is used in HPLC, is an ultraviolet spectropho tometer. Since, again, tiny absorbances must be measured, the spectrophotometer that is used most commonly is a double-beam unit (for stability), employing a filter with a band pass that peaks near 250 nm (for compactness liquid chromatography is only starting to come mtc routine' use in solving nmily t;c.il problems. Part uf the reason is that it has not been long since pumps and detectors have been brought under control, and it is even more recently that it has been possible to produce reliable and repeatable column packing materials. The latter is of extreme importance. Un less column packing materials are under good control, it is not possible to repeat with one instrument m one day an analysis that has been published on the basis of work done on another instrument on another day. Another reason for the delayed acceptance is, paradoxically enough, the bewildering variety of opportunities that are open in high pressure liquid chromatography. Essentially, there are four different techniques possible; liquid-liquid chromatography, described earlier, which is known as partition; liquidsolid chromatography, where the substrate is a solid, and which therefore depends on selec tive adsorption; molecular exausion, which represents an upgrading of gel permeation chromatography; and the well-known tech nique of ion exchange. Furthermore, there is on almost infinite choice of solvents and substrates. However, even now a substantial body of applications is emerging for which modem rTM" */ and high throughput of light). Again, the absorbance of the solvent is the reference ceil is compared to that of solvent plus sample in the sample celt UV spectro photometers of good design can measure absorption differences of 0.01$ with reasona ble accuracy. The search fur sensftivfty High pressure liquid dhromatograpby sys tems range in cost between 55,000 and $20,000. The price varies depending on complexity, convenience, versatility, and performance. Sensitivity is one of the present limitations of HPUC instruments, particularly wheacompared to gas chromatographs. For this reason, many other types of detectors are under in vestigation, including molecular fluorescence and flame ionization units. One can also imagine that infrared spectrophotometers and atomic absorption instruments (for metal ligands) could be used. Another approach is the automatic addition of a color-forming reagent to the eluted sample in order to enhance its detectability. This is done in amino acid analyzers. Despite its enormous promise, high pressure f. ANttALOiMV&C 2 3ETHOXV-4H YOROXY SENZALDEHYDi {fTHVL VANILLIN) X 4.HYOROXV a-WMtTHOXY SCN*ALOIHYQE IWTOYL VANtUiW f*WVU*0XY BENZOlC *ero ft-------- * ----is minutes iSQCSATie *0% CHC*s OKADIfur elution benefit* on state* b right in ffjWftltfoft of food flavoring compound** With isocratic (unchanging) solvent mixture at left, it is not possible to get a peak for component ho. 4, benzoic acid. With a gradient, dl four component* ant eluted and clearly separated. umi 4" u __ I V1--O u_ 16 mm--- GRADIENT tSUQCTAftf TO CHC*3 wSVWN CC 1718 " \ V Ir I } *:****..' / * t a. .. i *;*. . ....c .r r 1 i *n: tn t t bniii *....... fiYM highspeed liquid chromatography is the method of choice. In die production of polymers, highpressure molecular exclusion is used as the means to tell when die process should he stopped (conventional gel permea tion is too slow). A similar method determines residual monomers in polymers. Pharmaceutical houses use high pressure liquid chromalopaphy for fee determination of the presence and concentration of benzodiazopenes (tranquilizers) in tablets, thenothhvzme ( cough suppressant} in cough medicine, and for the measurement of de composition products in quality control of ston'd pluumaccuticals. Biochemical laboratories use it for the rapid rniriWi m Mi isolation of viruses (interestingly enough, purely by size) such as Markoffs virus iti chicken plasma, HPLC also is proving valuable for the analysis of dyestuffs and in termediates, which cannot generally be vaporized for use with gas chromatography. Also, it is possible, though not yet proved, to make the generalization that modem high pressure liquid chiomatogrnphs can repeat and improve any analysis now performed by ON paper or thin layer chromatography. One can visualize the Sat sheet used In the latter techniques being rolled up and inserted in a column, with an obvious gain in temperaturew control and Isolation from the atmosphere.CJ Speed, separation, and repeatability are aliQ <ilvAth and tlva*; i a fuvtVr Cciiriit in that tin* coUinms .u<* leusoable. SOLVENT POLARITY SCALE / Morovar. it h diincuU t* quanliiaU' the re sults of the simpler U dumpies, and such Solvent Viscosity E(AIO) fcf>. 20 ) UV Cutoff m (mu) Jt.v i^xs as scanners are expensive and hard to use. Thus, if quantitative results arc -dearotU modem liquid chromato graphs can even have a cost advantage. Don't dissolve the substrate To select the conditions for an IIPLC analysis, there are a few obvious basic condi tions. II a ivfraethe index detector is used, the solvent .should--as far as pcxssible--havc a substantially different index of refraction from tlie sample components of interest. For work with a UV detector, the solvent should have relatively low absmbance in the ultras iolet region. For obvious reasons, the statkmaiy phase, or substrate, should not be readily soluble in the solvent. To keep the solvent from dissolving the substrate, one is generally chosen to be a highly polar liquid, Fluoralkanes -0,23 n-Pomane 0M Hexane 0.00 l&ooctane 0.01 Petroleum ether 0.01 Cyclohexane 0.04 Carbon Tetrachloride 0.18 3u1yl chfonds 0.2$ i-Propyl ether 0.23 bPropyl chloride 0.29 Oenzene 0.32 Ethyl ether 0.38 Chloroform 0.40 Methylene chloride 0,42 Tetrahydrofuren 0.45 Meihylethyikctone 0.51 Acetone 0.55 Acetonitrile 0.65 l-propanol, n^propanol 0.52 Eihanol 0.85 `Methanol 0.95 Acetic achf Large Water Larger 0.23 0.33 0.3 0.3 1.00 0.97 0.47 0.37 0.33 0.65 0.23 0J7 0.44 0.35 0.3 0.32 0.37 2.3 1.20 0.60 1.26 MS 1.358 1.375 1.404 1.427 1.485 1.438 1.368 1.378 1.501 1.353 1.443 1.424 1.403 1.381 1.359 1.344 1.38 1.381 1.329 1.372 1.333 218 210 210 210 210 285 220 220 221 280 220 245 245 220 330 330 210 210 210 210 190 . while the other has very low polarity. Commonly, die substrate is polar and the solvent is not If it is the solvent that is polar, the technique is known as reverse-phase chromatography. Tables giving the polarities of different liquids, and hence their suita bility for use together, are widely published --and usually also show refractive index and UV transparency, An opportunity to increase the power of high pressure liquid chromatography, at the cost of complicating the iratnimcntation, is known as "gradient elution" Veteran gas opportunities that high pressure liquid properties chromatography offers, it is at least possible of some commercial solvents. Left hand that any analytical problem, no matter how numbers represent intractable, can be solved by the choice of the polarity measured proper column, substrate, and solvent More by interaction with aluminum oxide, over, again because of the complerities among RJ is refractive which one can wander, almost any work that is done probably is publishable. index. UV cutoff represents the wavelength above which Increasingly, however, useful general the solvent methods are emerging* As may be expected, is transparent. instrument manufacturers are falling upon 4 diromatographers will recognize this as die liquid chromatographic equivalent of column temperature programing. With gradient elution, an analysis starts out with Solvent A which, during the analysis, is gradually changed in a timed ami predictable manner to Solvent B. When gradient elution is properly used, it is possible to separate peaks which could not these with delight and giving them the widest possible drculadon. As a result high pressure liquid chro matography now is atthebeginning of a period of explosive growth. As routine analytical methexj* become increasingly available, high pressure liquid chromatographs will take their places beside gas dhromatographs in almost every type of analytical laboratory*Q be separated with a single solvent or solvent mixture. It also is possible to speed up die analysis for sample components which are not very soluble fa Solvent A* and to sharpen some of the later peaks, thereby increasing sensitivity. Gradient elution requires a second pump, as well as a solvent mixing chamber. Obviously, if a gradient consisting of two solvents is good, a gradient of three solvents is better, but fortunately, so far, only a few appear to have carried this bright idea into practice. It March Inin practice Up to now, the overwhelming majority of users of high pressure liquid cinematographs are In government, industry, md university research laboratories. Because of the variety of For abstracts of related articles from ABAC, NASA Regional Development Center, circle 678 on the reader service card. THE AUTHO RS Zone L. Bitterfidd is a chemistry graduate of Temple Vmvenity and has experience at Drew Chemical and Wilson Pharmaceutical. Hi* areas are moldy control, lipids, and GC. Now he is working at Perkin*Ebner with Herbert L. Kahn in HPLC.Kahn appeared in i*H in February at product manager for 9peciro&co\njf. Ha turn since moved to HTLG to be44where the action is" Zai*c, at left, is showing Herb where the >** sample goes in. OCC 1720 INDUSTRIAL RCSKAACM^UNS 1973 S3 >4 / I r ii l i i QPAUTt t&mnoi 300 pcwy 0 was the scrutinising eye of the alchemist From the Fisher Scientific Co* { cdteetim* interpreted % by I*ft staff artist, *\ 2*. , / 1 *AVvs ^3 s- t / ,* //' / i ***S*-> V ,i, * OTrfCm Uw/* ly--r-H---f-i product manager Fisher Scientific Co, 40 itt&usnuAL How<TMoMAT(X3iAFHYm^ for many industrial quality control ap plications is a story as Averse as industry itself. Rather than attempt to cover the entire - subject* this article will suggest some rules of thumb for the practical chemist to follow In assessing the applicability of gas chromatography to his quality control problems. Ex amples of procedures used in industry wilt be cited as further illustration of current Gas chromatography is accurate, precise, and rapid. With the advent of digital in tegrators and computerized data reduction, interpretation and quantitation of results has been sxmpKSecl The introduction of automatic sampling devices has permitted automation of many GC procedures* Hence, CC can replace lengthy or cumbersome bench chemistry methods* The problems of industrial quality control are numerous and varied. However a flexible GC instrument and an analyst with basic knowledge of GC technique can adapt procedures to solve almost any problem. Consider the typical problem of accurately determining die NIL. and CO* levels in im aqueous ammmtium carbonate solutions. Lengthy wet chemistry procedures including final titrations are necessary to report these compounds to the nearest 0,5* or better. Analysis time per sample exceeds 100 min. By employing the correct column stationary phase and GC inlet system, the gas chroma tographic determination of these components, including data interpretation, requires less than 8 minutes per sample* In this applica tion, the gas chromatograph is set up with a thermal conductivity detector, tube pyrolyser inlet system, and 7 ft (2*13 m) x 8 in. diameter stainless steel column packed with Porapak or equivalent stationary phase* The cohann is operated isothermalfy at 85 C with a helium carrier gas flow rate of about 40 ml/mm. The detector is maintained at 150 C to prevent any sample vapors from con densing while being detected. Sampling is done by transferring exactly 5 of solution into a small steel boat which is placed in side die pyrolyser tube and sealed. While carrier gas is sweeping through the pyrolvser tube into the packed column, the tube is heated rapidly to 1000 C. Under these conditions, die ammonium occ 1721 "-VT ,.i.r--, Jn-- dmrimt) dvUxi'>T. ninth ;!! r a irspt.iv ,<_ Kj iiiv txni1 nf nmiiKiimi'l i*. tiifKt mchil h<*vi' Tin-iv an* umiy similar analytic! quality control situations in the imngunic el unheal industry that ran be more easily handled by gas rhrnmutoguphy than by current wet techniques. At the Chemical Marrufaeturing Division of Fisher Scientific Co., quality control chemists rely on CC for various quality control determinations. Fishers 99 mole pure sol vents arc assayed by GC using either thermal conductivity or flame ionization detectors. The determination involves comparison of peak areas obtained from lot samples to those of standards having known mole purity. The following solvents are routinely assayed: acetone acetonitrile analine benzene n-butanol isobutanol chloroform toluene n,n dimethyl fonnamide 1, 4 dioxane ethyl acetate n hexane iso octane methanol carbon tetrachloride methylene chloride 2 propanol In some cases, GG is used to determine the level of certain impurities. In production of carbonate stotclrioroetrically decomposes to NH3, CO*, and 11*0. These gases are swept out of the pyrolyser boat into the column where they are separated and detected separately. A digital integrator automatically determines the peak areas. These areas am compared to areas produced by standard samples far quantitation using this equation: Area of std. __ Gone, of std. - Area of uribiown "" Cone. of miknown In this case, use of gas chromatography reduced analysts time from 100 aria to less than 8 min while maintaining die integrity of the results. More important, proper control of _high volume production facilities was made possible by fast reaction to results that were beyond specification. Employing GG allows corrections or alterations to be made in the production process without waiting 1-5 hours to find the product lot unacceptable. A noteworthy point about this example is that the sample is an aqueous, inorganic salt solution--not normally thought of as subject to GC detenaiantion. The use of a pyrolysis in let device permitted relatively easy and straight-forward GC work. A thermal con- formic acid, for example, it sometimes is difficult to prevent build up of acetic acid. At Fisher, GC procedures for the determination of acetic add impurity levels have replaced the old titration procedures. The GC pro cedure in this application offers three advantages. First; it is far less time-consuming and cumbersome, Second, it has specificity--it eliminates errors caused by other acidic materials present to smaller quantities. Where die titration would give total acidic im purities, GC quantitates die acetic acid in* dividually and unmistakably as a single, * specific peak on the chromatogram. Third, CC*s inherent sensitivity enables acetic add detection at lower levels than previously possible by titration. Turned an fey hydrocarbon* A similar procedure is employed to deter mine the level of extractable organic sub stances in hydrochloric acid. The HC1 k extracted with a suitable pure solvent and the extract is partially evaporated. The remainder OCCis examined on a GC column and the separated hydrocarbon impurities detected by stAftc*^u*E wn 41 *-+>( L"* ***- < J v-s **h *-%**% 4-#% diiiattci ui uuiiii y jjumia GAS CHROMATOGRAPHY it simply a meifcod tor separating mixtures into their individual components. As with other chromatographic techniques, the sample is placed in a mobile phase and carried across the surface of some stationary phase. The stationary phase is selected to intoract more strongly with some comport* cuts of the mixture than others and con sequently retard Hioir travel. This inter action, hosed on a difference of halting point, electronegativity, solubility, molec ular structure, and omer factors, causes the various components to pass through the stationary phase at different rates end thus effectively separates them. Gas chromatography, keeping to its name, employs a gas as the mobile phase. Samples are first converted true the vapor state. Next, they are swept by a constantly flowing carrier gas stream through a long narrow column which fa packed tightly with the desired station* ary phase, A gas chromatography system consists of several basic components Joined to* gather to: fl provide a constant flow of carrier gas. B permit introduction of sample va pors into the flowing gas stream. M. contain the appropriate length of narrow bore, packed column. B maintain the column at a constant temperature setficieift to keep alt samples in the vapor state. B detect tim components as they elute from the column and provide a readable signal proportional in alxe to die amount of component. Detecting devices can be universal like the Thermal Conductivity Detector, or specific such as the Fiame Ionization and Electron Capture Detectors. The signal, or chromatogram, consists of a series of peaks, one for each com ponent. The peak retentton time, or time required for elution of the component. Is used for qualitative identification of the component. The peak area is used as a relative measure of the amount of the component Utilizing appropriate quantitative standards, the ebrematographer can obtain precise and accurate quantitative data. Gas chromatography is applicable to any substance which can undergo con version to a stable, nonreactive vapor and then pass through a column. A vast array of organic materials as welt as the fixed gases lend themselves to GC determinatiofi. Most Inorganic compon ents are not amenable to GC work since they resist conversion to a stable, non-reactive vapor. Some inorganic sul fates and nitrates, by contrast, will con vert to stable fixed gases, and hence enable GC ctotenntoatlM, providing act indirect analysis. ---------------------- -- -- - -1 a highly sensitive fiame ionization detector (FID). The FID responds only to hydroear- bons and a well-designed FID will detect levels as tew as 30 ppb, . In addition to being highly sensitive to hy drocarbons the FID does not respond to water. In some instances, where die hydrocar bons are moderately soluble in water, direct water infection eliminate* the need lor ex traction. Even a considerable amount of water FTHOLYSIS of atnsswnk&m earbasuite is an excellent produces little or no response with the FID and, as a result, there is no interference with example of how GC even small hydrocarbon peaks. save* 0**4+ reducing Perhaps the most predominant use of gas a 100-rom operation to less than 8 min,, chromatography at the Fisher Chemical Division is for quality control of pesticide-free solvents. Following a procedure outlined by die Food and Drug Administration, samples from cadi lot of each solvent are analysed by gas cinematography coupled with an electron capture detector--the most sensitive method used today for detecting and determining halogenatcd pesticide residues. The detector sensitivity is adjusted so that i nanogram (IQ~dgram) of heptachior epoxide {chosen as an average standard by the FDA) per milliliter of solvent makes a half-scale deflection (50-division peak) on the chromatogram. To meet Fisher specifications, no solvent can contain existing impurities that produce a deflection of 1 mm on the chart. This means the impurities must be less than one part (heptachior epoxide) in 50-billion parts. The solvents assayed in diis manner include; acetone acetonitrile hexane methanol' benzene ethyl acetate methylene chloride carbon tetrachloride* 1-2-dichlon*tha t*<? n-pcntanc petroleum ether 2-propauoI __ `WWSTRIAL RESEARCH--1*73 I la ^ 1 {' illlM s ni Mill* iitK CO M,,,u!uio ti'u'u.tii stH'.u "I i'w tiiima ior GC *-n* r *aj i technique: S3 GC IYu(GkG VlNV tiliU*. jfif CC pmt edwvs air mmr jiemitive. 8 GC is mote specific, a GC procedures air simple and ravel)' cumbersome. Winn in me io decide between GC and bench chemist rv procedures, weigh the benefits lifted ahmc against the initial capital iKidity for tii* equipment. Gas chroma tographic systems c apable of a wide range of fjualiiv control Y\mk can lie chlairied for less than the cost of a technician for one year. Chromatographic variety There is certainly no shortage of gas chromatographs for the user to consider to day. A wide sek c turn of systems offering vary ing degrees of capability with one, two, and four columns, a choice of detector, and other components, plus all the sophistication and complexity one could want are on the market-each with its appropriate price. Since most GC procedures require the capabilities of a dual column unit, discussion here will focus on these systems. There are, however, simpler procedures which can be carried out on a single column instunient, but that's another subfeet What then are the features and performance qualities that a gas chromatograph should have to represent a good value for the analyst in quality control? Stability ranks as the most important single characteristic in selecting a gas chroma tograph for quality control work. Good stability means repeatable retention time (or elution time) and dm gives the analyst con fident peak identification and precise results. Retention time, in turn, is grossly affected by temperature and flow fluctuations. The highly stable GC instrument of choice, therefore, should employ a differential few controller for control of carrier gas to each column and should offer temperature stability of about 0.5 G ~- Most GC systems now available utilize state-of-the-art detectors and have adequate sensitivity to detect levels normally sought in quality control. A typical Same ionization detector, for example, will routinely detect less than 1 ppm of most hydrocarbons. Tho seeond-most-important characteristic is reliability'. The instrument must deliver consistent results around the clock. Instrument failure can delay an entire production facility and often can eliminate the only means of assaying product quality. Since down time is an inevitable occurence, however, the in strument should be easy to troubleshoot and repair. Before selecting GC instrument consider the following questions to help minimize down Ume brfoie it occurs, h the instrument * i I fo 3 J * ii j 1 modular? Docs it employ state-of-the-art /HXPNS!V solid-state electronics? Who services the chr&tttafo^rafth warranty, and what is their reputation? m use here it typical of units designed Several gas cliromatograpb manufacturers fee quality control have recognized the potential of GC in indus work, Its dual column trial quality control and have developed in system will accept struments specifically to suit quality control a variety of needs, A recently-introduced gas chroma sophisticated tograph has a versatile dual column system which features. multidctcctor capability* These include; dual flame ionization detector with standard dual channel electrometer; electron capture detector, supplied with an ECO Liaeaiizer (displays linear response to concentration ranges of 2 x I04); and dual thermal conductivity detector, filament or thermistor type. This choice of detectors combined with a large column oven introduces dozens of ap plications possibilities that were previously unavailable with an inexpensive GG system. THE AUTHOR Chromatographers can, for example, employ two dual detectors simultaneously enabling Patrick \V, Bytncs is gas chromatography product manager split effluent display (FID, ECD), or for the Analytical simultaneous TCD, FID operations, plus Instrument Div additional other operations. Fisher Scientific Co, Such a unit offers the temperature and flow stability needed for precise quality control He previously managed their applications laboratory, end is work. In addition, the choice of temperature a specialist programming provides the chromatographer in developing with all the versatility needed to accommo GC procedures. date analysts in almost any industry--chemi cals to textiles. This economical instrument in the $3,000 price range, makes available a quality instrument capable of adapting to & zr tn - P%7i'! I numerous QC procedures, including pyrolysis. r,;* 1~ With instruments of similar description and price coming on the scene, the quality con trol chemist can upgrade many of his current bench procedures; often reduce production costs; and always save analysis time. 3 :1 I Fm abstractv of related articles from ABAC, -OCC 1724NASA R<gional Development Center, circle mxmhrr 070 on tile reader service card. t* tmmtmM. mMAxcH-sw* yi dpi ay et me start by saying that this message equipment** as an isolated incident. Usually, Lis not being beamed out to the fat cats these days, a need indicates the purchase of who have a fully-equipped lab and/or theequipment and if the proper tools are selected capital equipment budget with elbow room to {and used properly) the needs will be ful spare. Actually, ftra really is a moot point, filled in a reasonable amount of time and -- for I suspect that all the fat cats died with the everyone will come out ahead. There should mid 1960s. be and is less of die "eraotionar purchasing No longer can a laboratory justify the pur which usually spelled trouble for the lab user, chase of a "tey~ which is fun to play with but fee instrument manufacturer, and ultimately does not justify its own existence on a month- for the management which okayed the original to-moofe basis. It has been observed that purchase* Dennis It Pare mdC*u*B*sm ** 8* ***q**e to the took of manager sevaration laboratory, but applies as well to project plaiming and evai to the chemists theinseivc^ Instrumentation or clatsieaf analysis? Let us examine, then, some representative Vartan Associate* Today, then, we have a much more sophisti approaches used to reach a sensible decision cated and discriminating group of people pur for purchase of dbromatogniphy instrumenta chasing ami justifying the purchase of labora tion. To begin wife, do you really need tory equipment instrumentation? This trend towards a tougher management Hus cannot be answered for all cases in line on purchase of equipment is even more general, but rather each case to be measured evident and significant in the smaller labora on its own merits. What one usually pur tories where funds are limited and competi chases these days in terms of chromatography tion for use of the funds is severe. What does equipment is not just a piece of hardware, but a person in such a laboratory do if he is rather a "capability.* This is often a com contemplating purchase of chromatography plex and expensive capability and fecrcfore equipment? requires some thought uud dfuii to make suie First of all, rarely does one simply "con the "capability provided" is well match-, d u ith template the purchase of chromatography the "capability needed/' *SEAACH-4VNE 1979 Modern hitsh-pcrfoniutnce liquid chronutographv, (liPJLC \ as ust*<i in Uh* $ln\nY*>iceuticat mduatrv provides several convincing arguments in favor of chromatography mstnmumtatnm over such wet chemical tech niques as thin-layer chromatography (TLC). for a typical analysis, a total of six man-hours would be allotted to the TLC technique whereas a total of one man-hour is all that is required for the HPLC technique includ ing precolumn work-up and post-separation data reduction. Not only docs one save time--but also new dimensions of resolution* precision, and ac curacy are now attainable. The same is true in the comparison of the gas chromatography of I7-kciosieroid$ in pregnancy wines* What n the choices? So, you're convinced that the added speed, sensitivity, through-put and resolution justify the capital expenditure to expand the capa bility of your limited budget lab. You now begin to explore die many pathways that could lead you to having such devices in your facility. If you simply walk in to your man agement and quote them typical prices "coldturkey" for a fully loaded chromatograph, you can almost be assmed they'll send you back to seek lower cost alternatives. ' Perhaps they will suggest that you pur- and P the TM chase a used model. Unless you are very luck}', that pathway is rarely worth pursuing. Used chromatographs are a tough commodity to find. It's something like buying md selling a used car. You must keep in mind there are several different terms used in describing the value: actual cash value, wholesale sell ing price, and retail buying price. Whereas your management expects you to find the model to match your needs at per haps 3S of the new price and only slightly used, you'll find a seven-year-old model sell ing at 70S of its full price and, upon dose scrutiny, it doesn't have your solid-state electrometer which is now considered stand ard equipment and the temperature ptogramer is a first generation design. There's even the problem of locating a used device that will meet your needs. The instru ment mamffacturers rarely offer used equip ment, for a variety of reasons. Used equip ment usually means a demonstration device used in an application lab for no more than one year. Usually, it is fully reworked in the factory before being shipped out, and then leaves with a new device warranty. This usually is a good Imv from (hr standpoint of niubditv and quality, hut from asi absolute dollar standpoint it will cost S5 to 95% of its original selling price. A well-designed, useful chromatograph should have no trouble lasting at least ten years. That means that a laboratory rarely will give up one of these devices short of some disaster. If they do, its Ix'cause they want or need a more capable device (how does your chemical problem compare with theirs?), or because they have had a lot of downtime with it The best possibility you have of obtaining a bargain is visiting a laboratory' which is being closed down. These days there are, admittedly, quite a number of these happen ings. Even then, the good capital equipment is reallocated to the other pails of the com pany before the outside public is allowed to look over the used equipment Assuming that you can find a used piece of equipment (a used high-performance liquid, chromatograph is impossible to find at this time), check carefully into a couple of other factors before you purchase it O Is the unit operational at this point? Will the seller aid you in making sure it is operational? 0 Is the unit amenable to servicing? O Are the replacement parts readily avail- f--*--....'m 1 ... -- ------- able today? Beware of the model whose manufacturer has ceased operation! LMSfvtff is ftr tax saving Perhaps your next option would be to try and lease acme equipment to avoid the capital outlay for the whole item at one time. This qptiem rarely turns out to be of any value in easing the original justification tor obtaining the equipment Its biggest value is as a tax writeoff benefit If your management is unwilling to lay out the original purchase price at this point dm idea of signing up for 36 monthly lease pay- r meats without any gain in equity doesn't appeal to them either. (No, Virginia, there is no 6-months lease, where you can send it back if you don't like it at the end of the short terml) If yours is a small independent laboratory, at this point of desperation you might con sider going to a private bank to see what they will do for you. Usually this is a very discouraging ordeal. Bankers take a very conservative stance concerning scientific equipment. This means you must have 502! of the purchase price available in assests _ OCC 1726 mimw. itrs C3 K-v. rr11form i,m >^>.3ort',nt cirouji .? cn EKV*r`* n !** ; ><i v ,,t> . tf'V* 7,5 cnrfrr' ttorrj.V.y riTO Q`iW. ll j *1 cf K.'I . rOMd,, ,t 1.11-r . ,"7jJ,y {* by cr* J V;%,*v ., t i >d r .#>ry w*iy <* v . *n^ * r,v It.lM \.c-v ` ..,7n. V. 0 c.. gram shows th* thcwj c.unman 17 kuostetotds ro WMW, nn-Myxad 41 TVS 'Vfw.mv*s. 4* f pregniruidtol. The interiMt surriitrd * chn? isferol. | ; 1 i3 % 1. Pre?'i4i*iechnl (TM^I 2. Ah-; t r vt r one < 1 X Pticvh'l4*:o'^p- (T&$j 4, Ochv<>o.pta^H*citffarta |TMS> 5. ChoU,:*s.ol (TMSi {imoffi;*! Stamford) 0 5 10 20 iw Conditions: timm tommlea detector; 6* x 1/4** *ass column with 1.5* OV-17 on 100/120 HP Chromoserb G: 200C; &2 at 30 inl/min. and the 50% you borrow should be paid back in no more than three years at stiff interest rates. Well, you're back to your own return on your assets calculation! Oftentimes the next idea you have con cerns buying components and potting them together yourself on a bare-bones allocation. The red flag really goes up here concerning man-power availability and hourly labor costs. You must make sure you are buying the state-of-the-art components first of all. Sec ondly, you need someone available in your facility who can lash it all together and make it work, and service it when it is down. A survey of a couple of the larger pharma ceutical firms which opted for this type of entree into high performance liquid chroma tography tadicates that this is not the best way for a fisraih-r< \fKnn:m<> organization in go. Ion'll find alter w couple oi yc.iu (Ua the jx'oph* you asMgmd to .isscnibk* <;:k1 tun the equipment have learned a lot alv-ut the technique, but meanwhile vour competi tors have turned out fmtr times the anah>%* workload on equipment which was purchased with a systems responsibility (by the manu facturer). Remember the commercial equipment is designed not only for ease of operation, but also very importantly, it is designed for serv iceability. Spending some time comparing mcan-time-to-failure and mcan-down-time of commercial system vs. put-together com ponents can be very revealing. Make tfi salesman work Finally, then, we come squarely back to the need for a systems responsibility. Justify your purchase on real need in your labora tory coupled with a capability which you don't possess at this time (or perhaps in not sufficient quantity), You should be taIfemg to a salesman in the early stages where he can help you define your needs in terms your management can easily recognize. He will also be helpful in referring you to current users of his equipment, com petitor equipment, and even basic-component equipment He can also put you in touch with other members of his own team (fust who else is on his team and whvP), Hell let you talk to his development engi neers and scientists who can tell you not only why a certain feature is available, but how a potential new feature could be added when the state-of-the-art advances. Concern ing features of equipment, don't foiget that the professional salesman can help you relate a hardware feature to a real benefit for you, the end-user, on your chemical problem. He also has access to an applications labora tory--a benefit which usually becomes ap parent after the sale, during the critical startup period of new equipment Remember, its not always fruitful to simply send in a customer sample to the applica tions laboratory and base your buying de- AUTOM4TJOM can cotne in various degree*. Deluding on your nerds, the more automation you have, the lower are ymr costs. Cost savings based on sample throughput Sttm instrument supervision Area measurement Composition calculation Report writing Total/sample Manual $ .50 3.00 1.97 1.00 S6.17 Operator Costs* integrator $ .10 .30 1-67 1.00 63.17 `Based on 10 p^aks, 10-minute chromatograms. $10/hour/operator Sjvmes/ye^/ Samptis/ti&y X savhigs/day X work fays/year Payoui/year System cost System cost Computer 9 .00 .30 .05 .05 S .45 OCC 1727 54 IMBUSTFUAt. ftSSSAROi-^UliE If** <Mm m the "beauty" of the chromatogram which it returns to you. Better that you ar range a visit to one of these laboratories and observe the equipment in action. Even tetter, get your own hands (or those of one of your laboratory personnel) on the equipment In the applications lab and operate if yourself. Keep in mind, also, that the applications staff probably will be available to you for consultation after the sale, a very useful service. They can provide you with a con tinuing source of technical data on the care, feeding, and expanded use of your equip ment Oftentimes this can be in the form of short courses, basic how-to manuals, and continuing bibliographies. There is also another group on the sales man's team that can be of vital assistance, the service engineers. At some time or other all equipment will develop a problem. The abilities of die service crew can substantially affect your minimum-down-time and frus tration level. This capability can rapidly overcome die difference in original purchase price of a complete commercial system vs. Ac put-together-yourself component kit. But there is one kiud of do-it-yourself that can make sense. A good compromise in the approach of putting components together yourself is to purchase a chromatograph which is designed in a modular concept. Finally, don't fail to consider automating features of a chromatograph. It may seem in compatible to consider an automated chro matograph when funds are limited. However, if a heavy workload is anticipated, automatic sample introduction and automated data han dling can, in fact, pay for themselves. Oper ating expenses are reduced by the manpower savings resulting from one or more of the following areas: instalment supervision and Atmins maintenance, quantitative calculations, and ^ repeat preparation. Faster sample through-put ^^ked^yeors makes it possible to reduce the number of for Varion Associates, chromatographs required for a given work load, sciences tn the Let your needs dictate your purchase applications tab, requirements. Justify these needs as credibly newlyrnplmd as you can define them. Seek assistance in at Hewlett-Packard:* defining these needs and requirements from Avondale Div. the instrument salesman ami his team of experts. Avoid Ac pitfalls of buying for emotional reasons or on strictly price com siderations. Determine how your chromatograph can and will do the work for you. Despite what some bankers might think, there are few investments that pay hade better or more dynamically than can a well designed chro matograph. * For abstracts of related articles from ARAC, NASA Regional Development Center, circle number 677 on the reader service card. oeet728- nnHismtAL nfARci4--auMi ms ESS 1 from 0.1 ul to 50 ml If you need to measure or deliver precise samples ... wfi hava the world's largest line of dfspensing devices from which you can choose. Our 700 mcroitiw syringes grew up m$% the QO industry ... and have become the standard measuring devices m laboratories throughout the world. Our 7000*$ contain the fuff volume in the needle. Our lOOO's have a Tefkm* dp for leak-tight seals for gases or liquids. And our new Sub-Microliter Liquid injector is a tapered capillary needle with high repeatability in O.t p\ volumes, a If you need to deliver samples anywhere from 0.1 /J to 50 ml, we have fust the syringe for you. Our syringes are described in our catalog... let us send you a copy. Write to Hamilton Company, Post Office Box 7500, Reno. Nevada 89b02. *ih&er?!i .H5H 0AT**** {f^rmm*b'***'Q**/$2f$$S9 4* *= 4 B V. Goodrich Chealeal Caapasy #tBB 6** ?** 9img - cumins, 0*10 (ni phm ji-92*-oiS8 *** i siS0 nitin ti Hiitilat. iHihtiMm * 5 lays ' Mr* Raymond Abramovitz Broker Chemical Corporation River Road Burlington, Maw Jersey 08016 Dear Ray: Rncloaed is a copy of a report "Progress is Vinyl Chloride Containment", which was distributed yesterday in a media briefing in Mew York. Aa a menber of the Vinyl Chloride/Polyvinyl Chloride Producers Committee of SPI, you may be interested in some of the things B.F.Goodrich has done in meeting the challenge of the vinyl chloride health problem. Yours very truly J.UMm/J* lAivV OCC 1730 1 ] hooker RifCO BMOON TO: Septeto* H.H. Kaster A. A. Katherine Subject: VCM NOMINATION - 1980 INTER-OFFICE MEMORANDUM File Ret: PLF-2-zc Date: April 30, 1979 From; Phillip L. Friedman Oiv./Dep*t: RUCO/New Ventures Location: Burlington This will confirm New Ventures* portion of the 1980 nomination for Shell VCM. Please allow 12.0 hW pounds of VCM for re-sale and PVC tolling. The total nomination including Burlington should therefore be 171 MM pounds, allowing approximately 180 MM pounds maximum under our contract. FORM NO. MMBM OCC 016394