Agilent Technologies G6600-90006 Bedienungsanleitung

Agile nt T echn ologi es Operat ion and Maintena nce Manual Agilent 355 Sulfur and 255 Nitrogen Chemiluminescence Detectors[...]

Notices © Agilent T echnologie s, Inc. 2007 No part of this manual may be reproduced in any form or by any means (including electronic storage and retr ieval or transla- tion into a foreign language) without prior agreement and written consent from Agi- lent T echnologie s, Inc. as governed by United States and internation al copyright laws. Manua[...]

Operation and Main tenance Manual 3 Wa r n i n g s English W ARN ING This symb ol on the instrume nt indicate s that the user should refer to the man - ual for op erating i nstruct ions. W ARN ING Any operation r equiring acce ss to the inside of the eq uipment, could resul t in injury . T o avoid potent ially dangerous shock, disconnect from power[...]

4 Operation and Mai ntenance Manua l W ARN ING Ozone is a hazardous gas and a strong oxidant. Exposure to oz one should be minimi zed by usi ng the inst rument i n a well- vent ilated are a and by venting t he exhaust of the v ac- uum pum p to a fume hood. The ozone generat or should be t urned off when t he instru ment is not in us e. W ARN ING Bu[...]

Operation and Main tenance Manual 5 Español W ARN ING Cualqui er oper ación q ue requiera acceso al interior del eq uipo, pue de causar una lesión. Para evitar pe ligros potenc iales, d esconectarlo de la alimentación a red antes de abrir el equipo. W ARN ING Para pr otección contínua c ontra el peligro de fuego, su stituir e l fusib le por u[...]

6 Operation and Mai ntenance Manua l Français W ARN ING Chaque opération à l'intérie ur de l'appareil, peu t causer du préjudi ce. Afin d'évite r un shock qui pourr ait être danger eux, discon nectez l' appareil du réseau avant de l 'ouvrir . W ARN ING Afin de protéger l'appareil continu ellement cont re l&apo[...]

Operation and Main tenance Manual 7 Deutsch W ARN ING V or dem Öf fnen de s Gerätes Netzst ecker zie hen! W ARN ING Für k ontinuierl ichen S chutz gegen B randgefahr dürfen bei Sicher ungswech- sel nur Siche rungen der gleic hen Stärke verwe ndet werden! W ARN ING Dies es Symbol auf dem Ge rät weist da rauf hin, das s der Anwend er zuerst das[...]

8 Operation and Mai ntenance Manua l Italiano W ARN ING Qualsias i interven to debba essere ef fettuato sullo strumento può ess ere potenzia lmente per icoloso a caus a della corrent e elettr ica. Il cavo di alimen- tazione deve essere staccato dallo strumento pri ma della sua aper tura. W ARN ING Per la prote zione da rischi da incendio in se gui[...]

Operation and Main tenance Manual 9 Dutc h W ARN ING Ieder e handeling binnen in het toes tel kan beschadiging ve roorzake n. Om ied - ere mo gelijk gevaarl ijke shock te ver mijden moet de aansluiting met het net verbrok en worden, vóór het ope nen van het toes tel. W ARN ING V oor een conti nue bescherm ing tegen brandge vaar , v ervang de ze k[...]

10 Operation and Mai ntenance Manua l The follo wing sym bols are used o n the eq uipme nt: Caution - Refer to manua l for operating in structions Caution - Ri sk of electrical shock . Caution - Ho t surface. Atención - V er docu mentación pertin ente. Atenci ón - Ries go de sacu didas eléctri cas. Atención - Superficie caliente. Atte ntio n -[...]

Operation and Main tenance Manual 11 Contents 1 Introduction 2 Syste m Descri ption Spec ifica tions 20 T echnical In formation — 355 SCD 20 T echnical Info rmation — 255 NCD 20 Physical Specificati ons 21 Theory o f Operat ion 23 Sulfur Chemi luminescence Dete ctor 23 Nitrogen Chem iluminescence Det ector 23 Dual Pla sma Contro ller 24 Descrip[...]

12 Operation and Mai ntenance Manua l 3 Installatio n Overview 40 Step 1: Selecti ng a Location 41 Power Req uirements 41 Figure 10 . Drawing o f the Detector wi th Dual Plasma Bu rner and C ontroller 42 Environ mental C onsidera tions 42 Combustion G as Requirement s 42 Step 2: Unp ack and In spect the Inst rument 45 Required Installatio n T ools [...]

Operation and Main tenance Manual 13 Packed Columns and Colu mns with an Outside Diameter > 0.8 mm 61 Step 10: Insta ll the T ransfer Line 62 4 Front Panel Controls and Initial St artup Detector Fro nt Panel Cont rols 64 Figure 21. Fron t Panel Cont rols 64 Power C ontrols 64 Displa y Output Co ntrols 65 Signal Control s 65 Dual Pla sma Contro l[...]

14 Operation and Mai ntenance Manua l 6M a i n t e n a n c e Pump Mai ntenance 82 T able 3. Opera ting Lif e of Co mponents for Ed wards RV 5 V acuum Pump 82 Cleaning t he Detector 83 Changi ng the Oil Mist F ilter (RV5) 84 Reaction Cell Cle aning 85 Figure 2 3. Reaction Cel l, PMT Housing and PMT Soc ket 86 Figur e 24. Reacti on Cell 86 Flow Sen s[...]

Operation and Main tenance Manual 15 7 T roubleshooting Solving Detector Pr oblems 106 Power Problems 107 Detector F use 107 V acuum Pump Fuse 107 Dual Pla sma Controll er Fuses 107 T able 4. Fuse s for 10 0 V , 120 V and 23 0 V V ersion s of 355 SCD an d 255 N CD 108 Figure 47. Fuse Positions on the Pow er Supply Bo ard 108 Ozone G enerati on Prob[...]

16 Operation and Mai ntenance Manua l[...]

17 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 1 Introduction This manu al will guide you in the ins tal lation, ope ration, and troublesh ooting of the Agilent 355 Su lfur Chemil umines cence Detecto r (SCD) and the Agilent 255 Ni trogen Chemilumin escence Det [...]

18 Operation and Mai ntenance Manua l[...]

19 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 2 System Description Spe cific ations 20 Theory of Op eration 23 Descrip tion of Majo r Compone nts 25[...]

20 Operation and Mai ntenance Manua l Specifica tions T echnic al Information — 355 SCD T echnic al Information — 255 NCD Sensitivit y * * Burner te mperature 800 °C, 80 SC CM air, and 60 S CCM hyrdr ogen, test compound dime thyl sulf ide in toluene . T ypical < 0.5 pg S/second ( signal to noi se 3.3:1 ) T y pic al Se lect ivit y g S/ g C &[...]

Operation and Main tenance Manual 21 Physical Specifications Power requir ements Dimensions and weight Repeatabil ity * <1.5% RSD 8 hours (~ the sam e in N and nitros amine) <2% RSD 18 hou rs (~3% RSD in nit rosamine mode ov er 21 hours) Gas fl ow thr ough Ozon e Gene rator 20-30 mL/min a t 3-6 p sig (inlet pressu re) T ypical reaction cell p[...]

22 Operation and Mai ntenance Manua l Dual Plasma Controll er Height: 5.0 in (12.7 cm) Wi dth: 9.5 in (24 .1 cm) Depth: 12.5 in ( 31.8 cm) W eight: 9. 9 lbs (4.5 kg ) Dual Plasma Burner Height: 12.3 in (31.2 cm) Diamete r: 4.0 in (10.2 cm) W eight: 1. 9 lbs (0.9 kg ) Oil Seale d V acuum Pump (RV5 ) Height: 10 .3 in (26.1 cm) Wi dth: 6.0 in (15 .2 c[...]

Operation and Main tenance Manual 23 Theory of Operation Sulfur Ch emiluminescence Detec tor The A gilent mod el 355 Sulfur Ch emilumin escence De tect or (SCD) is a sulfur-selective det ect or for gas chromat og raphy. Opera tion of t he SCD is based on the chemilum inescen ce (light-prod ucing reacti on) from th e reacti on of oz one wi th sulfur[...]

24 Operation and Mai ntenance Manua l Dual Plasma C ontroller The Dual Pl asma Con troller pro vides all op erational parameters o f the Dual Plasma Bur ner except for the Detec tor base temperatu re. The Det ect or base temp eratu re is co ntro lled b y cir cuitry in the G C. P arameters monitored o r regulat ed by th e Controller inc lude Bur ner[...]

Operation and Main tenance Manual 25 Description of Major Components Dual Plasma B urner The Dual Pl asma Burner c onsists o f a to w er assem bly that c ont ains an outer shea th fo r burn pr otecti on, a heati ng elemen t, thermocou ple, and comb ustion tube s. In the SCD, co nv ersi on of s ulfur containing com pound s to SO o ccurs wit hin t he[...]

26 Operation and Mai ntenance Manua l Figure 1 Cross -Secti on of the Dual Plasma Burner for the 35 5 SCD[...]

Operation and Main tenance Manual 27 Dual Plasma C ontroller The Dual Pl asma Con troller po w ers the Dual Pla sma Burner an d supplie s its gases. Hy drogen and o xidant should be provided at 25 p sig (1.72 ba r) and t he Contr oller i s plugged in to an appro priate A C electri cal outlet . The pa ramet ers monit ored o r regul ated by the Con t[...]

28 Operation and Mai ntenance Manua l temperat ure, hydrogen and o xidant f l o w rat es, and Bu rner p ressure . The tempera ture, ac tual p ressure , o xidan t and hydrogen f low rat es are se lected for displ ay by rotation of a 4-posit ion cont rol kn ob. P ow er , valv e operation, temperat ure wit hin se t-poin t range and fault cond ition s [...]

Operation and Main tenance Manual 29 Figure 3 355 SCD Left Side 5 4 6 6 1. Ozone Generator 2. High Voltage Trans form er 3. Photomultiplier Tube Sock et 4. Photomultiplier Housing 5. Reaction Cell 6. Vacuum Line 7. Particulate Filter 8. Pre-Ozone Restrictor 9. Post-Ozone Restrictor 10. Pressur e Trans ducer 8 7 9 10 1 2 3[...]

30 Operation and Mai ntenance Manua l Figure 4 355 SCD Ri ght Side LOAD NEUT P4 P5 WHT LOAD NEUT P6 P7 WHT LINE NEUT P2 P3 WHT AC OZONE GEN PUMP OUT TP2 TP3 TP12 TP8 TP9 TP1 0 TP11 HV /100 TP13 TP14 TP15 TP6 TP7 TP16 TP4 TP5 TP1 GND RV1 HV ELECTRONICS OZONE PUMP SIEVERS RESEARCH TP1 TP9 TP1 1 TO FRONT PANEL TP7 TP6 TP4 TP5 TP2 TP8 TP1 0 TP3 TP13 TP[...]

Operation and Main tenance Manual 31 Figure 5 255 NC D Left Side View[...]

32 Operation and Mai ntenance Manua l Pressure T ransducer V acuu m in the react ion cell is measur ed usin g a pres sure tr ansducer . The press ure of the reac tion cel l can b e monitore d fr om the fr ont panel and wil l typic ally ra nge fr om 5 to 10 tor r d epending on the type of vacuu m pump used, condit ion of t he chemic al (ozon e) trap[...]

Operation and Main tenance Manual 33 • Collection a nd transfer of the c ombustio n gases from t he Bur ner to t he rea ction cell. • Tr ansfer of ozone from t he ozon e genera tor t o the r eaction c ell. • Redu ction o f non -radiat iv e colli sional quench ing o f the emitt ing s pecie s in the c hemilumines cent reac tion cell. The higher[...]

34 Operation and Mai ntenance Manua l direct ly in front of t he phot omultip lier t ube (P MT). A red cut-of f f il ter be tween the reac tion c ell and the P MT sele ctivit y trans mits the lig ht fr om the nit ric o xide a nd oz one rea ction. Ef fi cient co mbusti on in th e ceram ic tubes and th e red cut -off f ilt er elimin ate inter ference[...]

Operation and Main tenance Manual 35 Figure 7 Schemati c for 355 SC D Ozone Ve nt C-Fi lt er Air H 2 Trap PMT Reaction Cell P Transfer Line Col umn Gas Chromatograph 355 SCD Dual Plasma Controller 25 psig max 25 psig max P NC S F.C. F.C. Dual Plasma Burner Mass flow Mass flow NC S[...]

36 Operation and Mai ntenance Manua l Figure 8 Schemati c for 25 5 NCD, in Nitro gen M ode Ozone Vent C-Filt er O 2 H 2 Trap PMT Reaction Cell P Transfer Line Colum n Gas Chromatograph 255 NCD Dual Pla sma Controller 25 psig max 25 psig max P NC S F.C. F.C. Dual Plasma Burner Mass flow Mass flow NC S Catalyst[...]

Operation and Main tenance Manual 37 Figure 9 Schemati c for 25 5 NCD , in Nitro samin e Mode Ozone Vent C-Filter O 2 * Trap PMT Reaction Cell P Transfer Line Column Gas C hroma tograp h 255 NCD Dual Plas ma Cont roller 25 psig max P NC S F.C. F.C. Dual Plasm a Burner Mass flow Mass flow NC S Catalyst Vacuum Pump *Or O 2 , He, N 2[...]

38 Operation and Mai ntenance Manua l[...]

39 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 3 Installation Overview 40 Step 1: Selecting a Location 41 Step 2: Unp ack and In spect the Inst rument 45 Step 3: Set Up the V acuum Pump 46 Step 4: Connect th e Power Cord 56 Step 5: Install the Dry Compressed Air[...]

40 Operation and Mai ntenance Manua l Overview Inst allat ion and s tar t-u p of th e A gilent 355 SC D or 255 NCD by a qu alif ied Agilent S ervice te chnician is reco mmended. If y ou choose to i nstall the detector y ourself, car efully read all of this c hapter prior to i nstallatio n of the instr umen t. Alt hough ever y rea sonab le safeguard[...]

Operation and Main tenance Manual 41 Step 1: Selectin g a Location The instr um ent shou ld be place d on a clean, unobstr uct ed sur fac e appro ximatel y 22" (5 5 cm) de ep by 10" (24 c m) wid e that can supp ort 44 pounds (19. 9 kg) in add ition to existi ng eq uipmen t. Fig ure 10 illustrate s the relatio nship b etween the m ajor sys[...]

42 Operation and Mai ntenance Manua l Environmenta l Considerations The instr ume nt should be operat ed in an en vironment wh ich is comfor t able f or hum an habi tation wi th reasonab ly co nstant tem per ature an d humidi ty. Operatio n of the instr um ent at elevate d t emperatur es (> 30 °C) may result in an incr eased back g round no ise[...]

Operation and Main tenance Manual 43 with air a s the o xidant in the SCD and o xygen as the o xidant in the NCD. F or th e SCD, detect or gase s must be sulfur free (<1 ppb) for proper Detec tor operat ion. In gene ral, bott led air is p ref erred to “house” air from a co mpre ssor because c ompressors t end t o generat e low e r quality ai[...]

44 Operation and Mai ntenance Manua l V enting G ases During nor mal op eration o f the GC wit h t he SCD, NCD, FID, o ther d ete cto rs and split/sp litless inlet p urge, some of the ca rrier gas and sample vents outsid e the GC. I n addit ion, the vacu um pum p will vent a small amo unt of ozon e and ot her com busti on products . If th e compone[...]

Operation and Main tenance Manual 45 Step 2: Unpack a nd Inspect the Ins trument Before unpacking box es , inspec t them f o r signs of physical damage. If damage is obse rved, phot ogr aphs sho uld be t aken in order t o ma k e a claim with the carrie r shoul d an y equi pment damage be f ound. Check contents o f bo x es agains t the shi pping do [...]

46 Operation and Mai ntenance Manua l Step 3: Set Up the V acuum Pump Initial co nnecti ons requ ire access to t he rear of the De tect or and t he vac uum pump. F ollow the inst allatio n instr uct ions for eith er the RV 5 Edwards pump or the o il-free dr y piston pump , depe nding o n you r configurat ion. Installing the Edwards RV5 Pump Oil-Sea[...]

Operation and Main tenance Manual 47 11 Remov e t he drain plu g and t he bonded seal from t he oil mist f ilt er . The bonded se al look s lik e a met al wash er wit h a black inner o-rin g. 12 Install the bonde d seal to t he oi l mist filter d rain adapte r . The drai n adapter looks lik e a drain plug wi th a small plast ic nozzle. 13 Scre w th[...]

48 Operation and Mai ntenance Manua l 26 The vacuu m pump should be placed wit hin app ro x imately 3 feet of th e Detector ( elevat ion not imp or tant), in ord er to conn ect the va cuum hos e fr om the ba ck of t he De te cto r to the ch em ic al t ra p. A ho se cla m p sh ou ld be placed o ver the hose , and t he hose sh ould be conn ected to t[...]

Operation and Main tenance Manual 49 Figure 11 RV5 Oil-Se aled V acuum Pump an d Associated T raps (Front Sid e) Figure 12 RV5 Oil-Se aled V acuum Pump an d Associated T raps (Back Side) Oi l mi s t filt er P o w er sw itc h M ode se l ec to r Edw ar ds EDW AR DS O i l return li n e C hem i cal Tr ap M ount i ng B racket B all as t contr ol B ar be[...]

50 Operation and Mai ntenance Manua l Figure 13 RV5 Oil- Se aled V acuum Pump and Assoc iated T raps (T op) P um p ex ha ust I nlet & v alve Ga s b a l l a s t Pu m p i n l e t O il fill c aps R et r ac t ab le handle Ch e m i ca l Tr a p NOTE Sometimes w ater condensation a nd accumulation are visible in the exhaust line. T his is normal. Howe[...]

Operation and Main tenance Manual 51 Setting the Gas Bal last Position (RV5 ) Set t he mode sele ctor ha lfwa y between t he High V ac uum mod e, the sm all 6 symbol (s ee Fig ure 14 ) and t he High Th roughput mode . Do not set th e mo de select or to t he High T hroughput mo de, t he large 6 symbol. The RV5 vacu um pump and t he Oil Drain Kit wit[...]

52 Operation and Mai ntenance Manua l • T o select n o gas b allast f lo w ( not re commended ), turn the rest rictor plate so that none of the ind entations ar e alig ned with the indentati on on th e side of t he oil retur n assembly. • T o select low gas ballast f lo w , turn the re stricto r plate so t hat t he sing le indent atio n on th e[...]

Operation and Main tenance Manual 53 10 Tighten the h ose cl amp lo cated on th e plasti c tube and the e lbo w barb end of the C hemical T rap. 11 Remo ve the pl asti c cap fr om the i nlet en d of th e Chemic al Trap. Ta king the clear en d of the va cuum ho se and an othe r hose cla mp attac h the v acuum hose t o the in let end of t he Chem ica[...]

54 Operation and Mai ntenance Manua l 6 Turn the s witc h on the va cu um pu mp to the On p os iti on. Figure 15 The Wel ch Dry Piston Pump Figure 16 Oil Drain Kit w ith Ballast Control R estric tor Plate Screws Indentation (Low Ballast) Indentati on (High Ba llast) Indentation (Alig nment G uide)[...]

Operation and Main tenance Manual 55 N o te th e p o sit ion of the oil le ve l i n the w ind o w aft er ope r at in g th e pum p f or several hours. For the next sev eral days of operat ion, rec heck the oi l lev el daily. If t he oil level is increa sing, w ater is accumu lating in t he oi l reser v oir . Conf irm tha t the wat er vap or is prope[...]

56 Operation and Mai ntenance Manua l Step 4: Connec t the Power Cord Connec t the p ump pow er cord t o t he female socket on t he ba ck of th e Det ect or (see Fig ure 1 7 ). The pump has a n On /Off switch locat ed on t he electric al moto r a n d t h i s s w i t c h s h o u l d b e t u r n e d O n . Do not conne ct to the A C po wer su ppl y at[...]

Operation and Main tenance Manual 57 Step 5: Install the Dry Compressed Air or O 2 Supply Connect a 1/8" OD Teflon (PF A) line fitted with a 1/8" brass Sw agelok nut from the AIR INLET at the r ear of the Detect or (see Figu re 17 ) t o a supply o f dr y compressed a ir or o xygen . The air regu lator located in side t he front door of t [...]

58 Operation and Mai ntenance Manua l Step 6: Ins tall the Si gnal Output Cables Signal outpu t cables are a vailable fr om Agilent as standar d equipment and can be used wit h mos t data system s. Conf irm tha t the out put cable supp lied is cor rect for your system . A sta ndard cable f itt ed w ith two crimp lug con nect ors is supplie d f or u[...]

Operation and Main tenance Manual 59 Step 7: Install the Dual Pl asma Burn er Re mo v e th e co v er pl at es f ro m th e De tec tor are a o f the GC to ex po se the h ole in to the o v en t hr ough whi ch a D etec tor is norm all y m ou nte d. If th e G C h as more t han one available De tect or po sition, pick th e most co nvenient one. Prepare t[...]

60 Operation and Mai ntenance Manua l Step 8: Install the Du al Pl asma Control ler P osition t he Controller such tha t the gas lin es from the Bur ner can be easily at tac he d to th e bac k o f th e C on tr oll er . Co nnec t th e C on tr oll er to bo th a hydr ogen source an d an oxidant sourc e, per St ep 1. Co nnect t he gas su pplies to the [...]

Operation and Main tenance Manual 61 Step 9: Instal l Column Connections The Bur ner operat es un der red uced pre ssure a nd th ere will b e a slight va cuum on th e end of t he colum n. If a higher o utlet pressu re for the colu mn outlet is desired , fused silica capillar y restric tors may be att ac hed to the end of the analy tical c olumn (bo[...]

62 Operation and Mai ntenance Manua l Step 10: Install the T ransfer Line Connec t the bla ck transfer line (ex tending from the side of the De tect or) t o t he top conne ctor on the B urner and tighten with a 3/8" open- end and 7/16" open-e nd wrenc h (backin g up t he union on t op of t he Bur ner t o prevent its posit ion f or m sl ip[...]

63 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 4 Front Panel Controls and Initial Startup Detect or Fron t Panel Co ntrol s 64 Detector Inte rface Setup 69[...]

64 Operation and Mai ntenance Manua l Detector Fron t Panel Contro ls As illustrated in Fi gu re 2 1 , the front pan el is div ided int o t hree sectio ns: signa l control , display outp ut cont rol, and pow er c ontrol. E ach sect ion is desc ribed belo w . All th e front panel LEDs ar e red in t he ON mode an d darkened in t he OFF mode ex cept f[...]

Operation and Main tenance Manual 65 Display Output C ontrols Signal C ontrols The SC D and N CD us e anal og ampl ifier cir cuitry f or the mea surement of the current p roduc ed b y the photomu ltipl ier tub e. Two Fr ont P anel Co ntro ls are u sed to a dj us t th e ou tp ut si gn al of the Dete ctor . Tur ns oz one gen erator ON or OFF . F unct[...]

66 Operation and Mai ntenance Manua l Dual Plasma C ontroller Controls The A gilent Dua l Plasma Co ntroller pro vides easy access to basic se ttings. The ba seline signa l from the SCD and N CD can be adjus ted from 0 to ±1% of the full scale recorder output u sing the offset cont rol. ( e.g. , +10 mV to -10 mV f or a 1 V full sca le setting). Th[...]

Operation and Main tenance Manual 67 Initial Startup V acuum T est With t he 1/8 " V alco cap on t he black PF A tra nsf er line s till in place a nd the a ir su p pl y to the o zo ne g en er ato r off, s et the in te rna l a ir re g ula tor t o 0 ps i ( ful l y count erclo ckwi se), and po wer on t he SCD o r NCD by plugg ing th e pow er cord[...]

68 Operation and Mai ntenance Manua l Reacti on cell pre ssure, wi th air to ozone genera tor OFF (0 psi setting o n inter nal regulator) and trans fer line capp ed: ___ _____________ ___ torr Tigh ten c onnectio ns if ne cessar y and ch eck to make sure p ressure st abilizes in th e expect ed regio n. If proper pr essure is n ot obt ained cont act[...]

Operation and Main tenance Manual 69 Detector Interfa ce Setup Initial Checkou t Careful att ention to eliminating leak s in t he Detec tor inte rfa ce will lead to bette r Dete ct or sensitivit y and easier troublesho oting if problems d evelop. 1 Check t hat t he gas conne ctions have been made cor rectly and t hat t hey are tight. 2 Plug the 3-p[...]

70 Operation and Mai ntenance Manua l Monitoring Oxidizer and Hydrogen Flow with the Dua l Plasma Controller Hydrogen will f low to the Bu rner on ly if the tempe rature is above 325 °C and the p ressure of the Bu rner is < 575 to rr . Turn ON the va cu um pu m p a t th e De tec tor and t he po w er to the Du al Pl a sma Contr oller . The po we[...]

71 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 5 Operation Start-Up Procedure 72 Detector Operati on 73 T yp ical Ope ratin g Cond itio ns 75 Detection Limi ts 76 Instrum ent Shut- Down 77 Spe cial Op era ting M odes 78[...]

72 Operation and Mai ntenance Manua l Start- Up Procedure 1 Tu rn o n the G C and se t the c arr ier f lo w rat e. 2 Turn on the h ydr o gen and o xyg en to th e Du al Pl as ma Co ntr oll e r . 3 Turn the Detector fr om ST ANDB Y to ON. 4 Press t he PUMP butt on until t he red LED illuminat es. Make sure the vacuum pump is ru nning. 5 Tu rn on t he[...]

Operation and Main tenance Manual 73 Detector Operation Detector Stability and Response The tim e requ ired for syst em st ab ilization varies de pend ing on t he applica tion, syste m cleanlin ess, pres ence of ac tive site s and ot her fact ors. Us eful results coul d be generat ed wit hin 30 minut es of st ar t- up, esp ecially wit h a previou s[...]

74 Operation and Mai ntenance Manua l Contaminated Gases The use o f clean gases for th e 355 SCD is es sential for opti mal per formanc e. High purity gases (99.999% pu re or better ) are advised. Sulfur and other contaminants from gases ma y accumulate in the colu mn and bleed out o ver time d esensitiz ing t he t ubes and causing elevate d base [...]

Operation and Main tenance Manual 75 T yp ical O perating C ondit ions The Con troller is calibrat ed at t he fact or y f or f lo w rat es to deliver gas in sccm units . The f ollo wing table summar izes the typical oper ating condit ions: Ta b l e 1 T yp ical Ope ratin g Cond itio ns Condition SCD NCD Dete ctor Pressu re (T orr) 4-8 (6 -12 * ) * O[...]

76 Operation and Mai ntenance Manua l Detecti on Limits The follo win g ta ble lists t he detect ion limi ts which can be expect ed for typical chromat og raph ic co nditions , assu ming p roper operatio n of t he Det ecto r and chromat og raphic syst ems. Ta b l e 2 Expected D etection Limits fo r Chromatographi c Conditions T ype of Injection V o[...]

Operation and Main tenance Manual 77 Instrum ent Shut -Down Daily Shu tdown 1 T oggle off the ozone genera tor . 2 Tu rn of f the air r egulat or (count er-clockwise) , locat ed inside Dete cto r door . 3 Tog g l e p owe r t o " s t an d - b y . " 4 Lea ve the vacuum pum p and Dual Plas ma Contr oller op erating at all time s. Complete Sh[...]

78 Operation and Mai ntenance Manua l Special Operatin g Modes Using the 255 NC D in Nitrosamine Mode By de fault, the 255 N CD is confi gured to de tect nitr ogen. T o change fro m nitr ogen to nitr osamin e mode, fir st turn off and unpl ug the Cont rolle r . Remo ve the co ver , find jum per P6 and the posi tion s label led Hi gh Set point and L[...]

Operation and Main tenance Manual 79 can be achiev ed by elimi nating the lo wer p lasma. Thi s is acco mplish ed by plugging t he side p or t of th e splitter fittin g and t eeing th e air int o th e lo wer h ydr ogen line, m uch lik e the c onfiguration use d f or Nitr osamine analy sis as sho wn in Figu re 9 . A slig htly lo we r air f lo w rate[...]

80 Operation and Mai ntenance Manua l[...]

81 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 6 Maintena nce Pump Mai ntenance 82 Clea ning th e Detec tor 83 Changi ng the Oil Mist F ilter (RV5) 84 Reaction Cel l Cleaning 85 Flow Sen sor Cali bration 88 Detector Sensi tivity 89 Assembling the Dua l Plasma Bu[...]

82 Operation and Mai ntenance Manua l Pump Maint enanc e T o ma intain opt imum perf ormance of the Agilent 355 SC D and 2 55 N CD, routine re placemen t of the c hemical tra p (for ozone dest ruct ion), oil coales cing filter and oil (Edward s oil-s ealed pu mp onl y) is necessary. Ref er to Table 3 f or th e expect ed life span of each repl acem [...]

Operation and Main tenance Manual 83 Cleaning the Detector Y ou can cl ean the e xternal hous ing o f the Detector w ith a dam p cloth usin g wat er or n on-abr asive cleane rs. T u rn o ff pow er t o t he D etect or a nd d isconne ct it fro m main po wer prior to cleaning. D o not spra y liquids directl y on the Detector . Wipe dr y with a clean, [...]

84 Operation and Mai ntenance Manua l Changi ng the Oil Mist Fi lter (RV5) The oi l mi st filter o n the RV 5 pum p ha s tw o co mp onents: the c harco al odo r fi lter and t he oil coa lescing f ilter eleme nt. T o replace t he f ilters, di sassemb le the oi l mist f ilter assembly wit h th e 4 mm long-hand led allen wre nch (provided). The smalle[...]

Operation and Main tenance Manual 85 Reacti on Cell Cleaning Over time, the reaction cell an d UV pass f ilt er (SC D) or I R pass filt er ( N CD) will d ev elop a build- up of mater ial which should be remo ved f or optimu m sensitivi ty. The clea ning sche dule depends upon De tecto r use and t he nat ure of the a nalyses; how ever , it is recomm[...]

86 Operation and Mai ntenance Manua l 6 Use a 7/64" Alle n wren ch to rem ov e the three mountin g scre ws fr om the reacti on cel l. Slo wly pull the reacti on cell back from the PMT housing. The optic al filter is lo cated betw een the reacti on cell and the PMT h ousing. Re mo ve the opt ic al fil ter fr om th e h ou s in g b y ti ppi ng u [...]

Operation and Main tenance Manual 87 8 Clean any deposi ts on t he optical f ilter using a so ft clo th or Kimwipe dampened wit h met han ol or deioni zed (D I) wat er . D o not leave fing erprin ts or fi bers on t he cle aned f ilter . Deposi ts inside t he rea ction ce ll can be clea ned in the same manner , ho we ve r , care must b e tak en to a[...]

88 Operation and Mai ntenance Manua l Flow Sensor Calibr ation The h ydrogen and o xidan t f low sensors installed in the Du al Plasma Co ntro ller hav e ver y good repe atab ility , but sign ific ant non-linea rity. They hav e each been fact or y calibrat ed at th e midrange f lo w rate (50 SCCM) using an NIST trac eable flo w meter . Ov er the t [...]

Operation and Main tenance Manual 89 Detector Sens itivity Dete ct or sensit ivity is an indi cato r ref lecti ng the p er formanc e charac te ristics of a given syst em, and is a usefu l tool t o det ermin e when Det ect or mainten ance i s warranted. Sensit ivity is typ icall y rep or ted as a minimu m detectio n limi t (MDL) as calculat ed from [...]

90 Operation and Mai ntenance Manua l Assemblin g the Dual Plasma Burner for Component Replacement with the SCD The f ollo wing pr oced ure ca n be us ed to ass emble the Dual Plasma Burner f or use wit h t he SCD or f or repl acement of Burn er componen ts, such a s ceramic tubes. Refer t o Fig ure 1 o n page 26 f or proper part nomenclature. 1 Sl[...]

Operation and Main tenance Manual 91 7 P osition t he up per cer amic tube in to t he long ax is of th e splitt er fi tting so tha t ab ou t 4 m m o f i t ex te nd s p as t the to p o f th e fit ti n g. Sl i de the 0. 0 54 " I D do ub le tap er ed f errul e o v er the upp er ce ra mi c t ub e. Ge nt l y h old ing thes e par ts so t hat neit he[...]

92 Operation and Mai ntenance Manua l 8 Appro xima tely 1.5 cm of t he large c eramic tu be should ex tend abov e th e top of the q uar tz heat er asse mbly. Slide a 1/4 " Swagelok n ut ov e r the la rge ceram ic tube and the n also slide a 1/4" ferr ule over the tube (f lat sid e on back o f t he n ut). 9 Holding t he split ter f itting,[...]

Operation and Main tenance Manual 93 adapter , rotate this fit ting s o that the bra zed H 2 line is aligned 18 0 ° (opposit e) from t he oxidizer Inlet po rt. 12 Making su re t hat t he Bur ner inlet fi tting does n ot loose n, use a 1/2" wren ch on a f lat of the tapered un ion fitti ng and 9/ 16" wr ench on the 1/4" Sw agelok nu [...]

94 Operation and Mai ntenance Manua l 15 Car efu lly b end th e H 2 line into positi on so that the 1/ 16" V alco nut and ferr ule can be scr e wed int o the sid e por t of th e splitt er f itting. T ight en th e connec tion of th e H 2 lin e to the sp litter fit ting using a 3/8 " wren ch on the vertic al f l at of the sp litter fitti ng[...]

Operation and Main tenance Manual 95 Assemblin g the Dual Plasma Burner for Component Replacement with the NCD The f ollo wing pr oced ure ca n be us ed to ass emble the Dual Plasma Burner f or use wit h t he NCD or for replac ement of Bu rne r component s, such as ceram ic tubes. Refer t o Fig ur e 2 on p a g e 2 7 fo r p r o p e r p a r t n o m e[...]

96 Operation and Mai ntenance Manua l 8 Inser t t he low er burner tube int o th e cent er of the quar tz tu be and f inger tigh ten the h eater sw iv el nut o nto the tapered union fitting, then ti ghten an additio nal 1/4 tu rn m aking sur e not to br eak th e quar tz tu be. 9 T o begin t he f inal tig hte ning, use a 7/1 6" wrenc h and 5/16[...]

Operation and Main tenance Manual 97 10 Using a 5/8 " wrench on the he ater swivel nut an d a 1/2" wren ch on one o f the f lats of t he t apered union f itting, ti ghten t he hea ter swi v el nut one-qu ar ter tu rn pa st fin ger-tight. Using a 5/16" wrenc h on t he ¼" Bur ner adapter , rotate this fit ting s o that the bra ze[...]

98 Operation and Mai ntenance Manua l T ube Replacement for the SCD The Bur ner has two com bustion tubes t hat requ ire replac ement: the up per ceramic tube and the Large Ceramic T ube . Generally th e tubes shou ld be replac ed only if sensitivi ty decre ases. The “T roubleshootin g” cha pter p ro vides additio nal infor matio n to assist in[...]

Operation and Main tenance Manual 99 10 Holding t he split ter f itting, gently inser t t he upper c eramic tu be into the large ceramic tube coax iall y , to a v oid pla cing stre ss on the fr agile upper ceram ic tube. Lo wer t he splitt er f itting in to pla ce to eng age t he th reads of the 1/4 " Swa gelok nut. Tig hten finge r -tig ht. 1[...]

100 Operation and Mainte nance Manual 15 Appro xima tely 1.5 cm of t he large c eramic tu be should ex tend abov e th e top of the q uar tz heat er asse mbly. Slide a 1/4 " Swagelok n ut ov e r the la rge ceram ic tube and the n also slide a 1/4" ferr ule over the tube (f lat sid e on back o f t he n ut). 16 T o b egin the f in al alig nm[...]

Operation and Main tenance Manual 101 nu t o f the Bu rne r ada pter to ti gh ten the ta pe re d u ni on fi tt ing one -q ua rter turn pa st finger -ti ght. 19 Ro tate the q ua rtz he at er as se mb l y s o tha t th e th ermo co up le an d h eate r leads ar e in the same pl ane and poi nted in the sa me directi on as the peg on the Bu rner inle t f[...]

102 Operation and Mainte nance Manual T ube Replacement for the NCD The Bur ner has o ne quar tz combus tion tube t hat req uires re placemen t. Genera ll y t he tube sh ould be repl aced only if sensit ivity dec reases. The “Trouble shootin g” chapter pro vides addit ional in formati on to assist in determini ng whether tube replac ement ma y [...]

Operation and Main tenance Manual 103 10 Inser t t he low er burner tube int o th e cent er of the quar tz tu be and f inger tigh ten the h eater sw iv el nut o nto the tapered union fitting, then ti ghten an additio nal 1/4 tu rn m aking sur e not to br eak th e quar tz tu be. 11 T o begin t he f inal tig hte ning, use a 7/1 6" wrenc h and 5/[...]

104 Operation and Mainte nance Manual 15 The ass embled Bu rner is now ready for re -inst allation on th e GC, inc ludin g column placemen t. Figure 45 NCD T ube R eplacemen t Detail Figure 46 NCD T ube R eplacemen t Detail[...]

105 Agilen t 355 S ulfur and 2 55 Nitr ogen Chemil uminesc ence Dete ctors Opera tion a nd Mai ntena nce Ma nual Agilent T ec hnologies 7 T roubleshooting Solving Detector Probl ems 106 Power Problems 107 Ozone G enera tion Prob lems 109 Response Problems 11 1 T emperature Re ading Pro blems 112 Diagn osing Gene ral Pro blems 113[...]

106 Operation and Mainte nance Manual Solving Detec tor Problems A basic un derst and ing of th e Detec tor helps one syst emat ically diagno se and sol ve Detector pr oblems . Man y sym pt oms ma y be cause d by more than one problem and t hes e are t he most di ff icult t o troublesho ot. It sho uld be point ed out, ho we ver , t hat anal ysis of[...]

Operation and Main tenance Manual 107 Power Problem s The f irst st ep in t he deter min ation of a p o wer re lated p roblem is to verify po we r to the p um p, C on tr oll er , and Det ec to r it s elf . The in abil ity to es tab li sh po wer may be as trivia l as a blo wn fu se. F use requirem ents an d posi tions on th e Detec tor ar e indica t[...]

108 Operation and Mainte nance Manual 3 Remov e the o ld fuses from t he holder an d replace wi th new fuses. If the C ontr oller s till do es not po we r on after repla cing the f use, co ntact Agi le nt . Consult Table 4 f or the appr opriate replacem ent fuse . T able 4 Fuses for 100 V , 120 V and 230 V V er sions of 355 SCD and 255 NCD 100/120 [...]

Operation and Main tenance Manual 109 Ozone Generation Problems F ol lo wi ng the v er if ic ati o n o f p o we r to the in st rume n tal co mp onen ts, the next step in tracing a problem is the det er mination of o zone productio n. With t he ozone t ogg le of f an d the va cuum pump on , read t he sign al output on the fron t of the De tector . T[...]

110 Operation and Mainte nance Manual Plugged Restrictor Lines Plugged restrictor lines ar e v erified b y turning o f f the air /o xyge n regulator located i nside the do or of the Detector and obs erving little or no change i n the pressu re as indi cate d on th e regulat or . T he plug ca n be locate d in eit her th e pre-o zone rest rict or or [...]

Operation and Main tenance Manual 111 Respon se Proble ms Lo w or no res ponse problem s are the most dif fic ult to troubleshoot o n the Agilent S CD and N CD as the y ma y aris e fro m one sour ce or a combin ation o f sources. Primarily , respo nse problems are due to combustio n problems, an d Burner integrit y shou ld be inv esti gated firs t.[...]

112 Operation and Mainte nance Manual T emperature Reading Prob lems No rmally , the contr oller displa ys the burner tem peratur e set -point . F or diagno stic purp oses, a switch in t he cont roller (JP2) can be posit ioned t o allow the dis play of th e actual t her mocoup le temper ature rea ding. When the ac tual temp eratu re and se t-poin t[...]

Operation and Main tenance Manual 113 Diagnos ing General Prob lems Ta b l e 5 T roublesho oting D etector Is sues Problem Possible Cause Diagnosis Corrective Action No Resp onse No ozone Little or no diff erence in output sign al between ozone ON vs. OFF . T y pically the backgr ound sign al will be 0.3- 0.8 mV highe r wit h th e ozone ON. Contin [...]

114 Operation and Mainte nance Manual Low Re sponse Con tamina ted cer amic tube s. If there does not app ear to be a leak, then th e tubes shou ld be in spected . Con tam inat ion can res ult from co lumn bl eed, sam ples which may co ntain volati le metal complexes, an d large injection s of coke forming hydroc arbons. Replac e tubes. W andering [...]

Operation and Main tenance Manual 115 Burner F ault Cycles . (off an d ON) Cracke d tube. Pres sure incr eases >525 t orr , Bu rner faults. Cycle repeated as tempera ture and pr essure reset. Replac e broken tube s. Burner F ault Cycl es (off and ON) Leak in Burner . Pressure increases >600 t orr , Bu rner faults. Cycle repeated as tempera tu[...]

116 Operation and Mainte nance Manual Ta b l e 7 T r oubleshoo ting Burner Issues Problem Possible Cause Diagnosis Corrective Action Fuses Blow on Startup Sh orted heate r element . Inspect for expo sed wires or broken insu lation around wire leads. Meas ure resi stan ce le ads , shou ld no t be 0. T ake Bu rner top o ff and reseat insulati on arou[...]

Operation and Main tenance Manual 117 Index C Calibration of Flow Sensor , 88 Ceramic T ube Replacemen t , 98 Column Insertion Distance , 61 D Detec tion Li mits , 76 Detec tor cleaning , 83 disp lay o utput co ntrol s , 65 initial check , 69 operat ing condit ions , 75 operation , 73 power controls , 64 schematic, NCD , 36 schematic, NCD (nitrosam[...]

© Agilent T echnologies, Inc . Printed in USA, J une 2007 Agilent T echnologie s[...]