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65 6 6 6.7 68 6 9 Stnp chart recorder A recorder IS strongly recommended for furnace work so that there wIll be a permanent record and any problems WIth the analysIs such as dnft, mcomplete atomIzatIOn, losses durmg charnng, changes m sensItivIty, etc, can be easIly recognIzed PIpets MICrolIter WIth dIsposable tIpS SIzes can range from 5 to 100 mICrolIters as reqUIred NOTE 7 PIpet tips whIch are whIte m color, do not contam CdS, and have been found SUItable for research work are avaIlable from Ulster SCIentIfic, Inc 53 Mam St HIghland, NY 12528 (914) 691-7500 Pressure-reducmg valves The supplIes of fuel and OXIdant shall be mamtamed at pressures somewhat hIgher than the controlled operatmg pressure of the mstrument by SUItable valves Separatoryflasks 250ml,orlarger,forextractIOnWIthorganIcsolvents Glassware All glassware, lmear polyethylene, polyproplyene or Teflon contamers, mcludmg sample bottles, should be washed WIth detergent, rmsed WIth tap water, 1 1 nItric aCId, tap water, 1 1 hydrochlonc aCId, tap water and deIOnIZed dIstIlled water m that order [See Notes 1 and 2 under (41) concernIng the use of chromIc acId and the cleanIng procedure] 6 10 7. Reagents BorosIlIcate glass dIstIllatIOn apparatus 71 DeIOnIZed dIstIlled water Prepare by passmg dIstilled water through a mIxed bed of catIOnandanIonexchangeresms UsedeIOnIzeddIstilledwaterforthepreparatIOnofall reagents, calIbratIOn standards, and as dIlutIOn water 72 NItnc aCId (conc) If metal Impunties are found to be present, dIstIll reagent grade nItnc aCId m a borOSIlIcate glass dIstIllatIOn apparatus or use a spectrograde aCId CautIOn DIstillatIOn should be performed m hood WIth protectIve sash m place 721 NItnc ACId (11) Prepare a l l dIlutIOn WIth deIOnIZed, dIstIlled water by addmg the conc aCId to an equal volume ofwater 7.3 Hydrochlonc aCId (11) Prepare a l l solutIOn of reagent grade hydrochlonc aCId and deIOnIzed dIstIlled water If metal Impunties are found to be present, dIStIll thIS mIxture from a borOSIlIcate glass dIstIllatIOn apparatus or use a spectrograde aCId 74 Stock standard metal solutIOns Prepare as dIrected m (8 1) and under the mdiVIdual metalprocedures CommerCIallyavaIlablestockstandardsolutIOnsmayalsobeused 75 CalIbratIOn standards Prepare a senes of standards of the metal by dIlutIOn of the appropnate stock metal solutIOn to cover the concentratIOn range deSIred 76 Fuel and OXIdant CommerCIal grade acetylene IS generally acceptable AIr may be supplIed from a compressed aIr lIne, a laboratory compressor, or from a cylInder of compressed arr Reagent grade nItrous OXIde IS also reqUIred for certam determmatIOns Standard, commerCIally avaIlable argon and nItrogen are reqUIred for furnace work 77 SpecIal reagents for the extractIOn procedure 7 7 1 PyrrolIdme dithIOcarbamic aCId (PDCA) "see footnote" Prepare by addmg 18 m1 of analytical reagent grade pyrrolIdme to 500 ml of chloroform m a lIter flask The name pyrrohdine dithlOcarbamic aCId (PDCA), although commonly referenced m the SCIentIfic literature IS ambiguous From the chemIcal reaction of pyrrohdme and carbon dIsulfide a more proper name would be I-pyrrohdme carbodithlO1C aCId, PCDA (CAS RegIstry No 25769-03-3) MET ALS-lOPDF Image | Methods for Chemical Analysis of Water and Wastes
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