mi22-€581 A, SERVICE MANUAL HVG-1 HYDRIDE VAPOR GENERATOR SHIMADZU CORPORATION ANALYTICAL INSTRUMENTS DIVISION KYOTO, VapANoc) v ed 7. CONTENTS Installation 1.1 Tools and Parts Required for Installation... 1.2 _ Installation Procedures... Performance Check .. 2.1 Maximum Pump Output. 2:2. Flashing Check......... 2.3 Pressure Switch Check... 2.4 Sensitivity and C.V. Value Check Troubleshooting .... Procedures of Adjustment 4.1. Tools and Materials Required for Adjustment... 4.2. Flow Path Adjustment 4.2.1 Argon Gas (supplying gas) Flow Adjustment 4.2.2 Operation Check of Pressure Switel 4.2.3 Flash Timer Setting 4.2.4 Performance Check ... Construction and Principle of Operation Reagent Preparation 6.1 Tools Required for Reagent Preparation 6.2. Reagents to be Purchased . 6.3 Reagents Required for Adjustment and Inspection and Their Quantity 6.4 Preparation of Reagents 6.5 Cautions for Using Reagents ... Parts List Electric Circuit Diagram .. Flow Path Diagram .. BD Aannnunn © HNHNKHNKN wordy a41. Installation 1.1 Tools and Parts Required for Installation (1) Volumetric cylinder (10ml) 1 (2) Stop watch 1 (3) Reagents Sodium borohydride solution (0.4% NaBH, + 0.5% NaOH) 500 mi Hydrochloric acid (5M HCl) 500 ml (4) Sample Arsenic standard solution (AS_10ppb) 500 ml (5) Distilled water Notes: 1) Sodium borohydride solution and arsenic standard solution are to be prepared immediately before starting the measurement, Stale solution may reduce the sensitivity. 2) _ For the method of preparing reagents, see ‘6. Preparation of Rea- gents"’ of this manual and ‘4, Preparation” of the Instruction Manual. 1.2. Installation Procedures See ‘*2. Installation’’ of the Instruction Manual.2. Performance Check 2.1 Maximum Pump Output Run the pumpin reference to ‘4.1 Preparation” of the Instruction Manual and turn the speed control knob to the maximum. Let the pump aspirate distilled water from a volumetric cylinder to check flow rate specified below. The measurement is to be started after 10 min. run. (1) Reagent 3.0ml/min or greater (for NaBH,, HCl) (2) Sample 8.0ml/min or greater 2.2 Flashing Check (1) Set the speed control knob to ‘*30°* and press the flash switch, (2) Make sure that the FLASH lamp lights up, the rotor runs at the maximum speed for about 20 ~ 25 sec, and then, returns to the initial speed. 2.3. Pressure Switch Check (1) Make sure that when the gas supply pressure is set to below 2.8 + 0.2kgf/em’, the PRESSURE lamp lights up and the pump rotor stops. (2) Make sure that when the gas supply pressure is raised again to 2.8 + 0.2kgf/cm’ or higher, the PRESSURE lamp goes out and the pump rotor starts to run. (3) After finishing these checks, set the gas supply pressure to 3.2kgf/cm*. 2.4 Sensitivity and C.V. Value Check (1) Connect the Hydride Generator HVG-1 to the Atomic Absorption Photometer and measure As 10 ppb solution 5 times with the following condition. Sample: As 10 ppb, added with 1M HCI Reagent: acid ... 5M HCI reducing reagent ... 0.4% NaBH, + 0.5% NaOH soln Flame: CH, 2.0 ml/min Sample flow rate: 5.5 ml/min INTEG TIME: 10 sec REPEAT: 5 times (2) Make sure that the sensitivity and C.V. value are as given below. Sensitivity: 0.25 Abs or more CV. 5% or less3. Troubleshooting Troubles Causes Countermeasures 1. The instrument is not Fuse blown out. Replace fuse. energized. Gas supply pressure too low. (PRESSURE lamp lit) Raise the gas supply pressure PRESSURE switch defective. Replace PRESSURE switch. coe Motor or control PAC Replace motor or control PAC. defective, Timer defective. Replace timer. Timer not set. Set timer. 3. Flash switch disabled, Timer defective. Replace timer. Flash switch defective. Replace flash switch. 4, Sensitivity too low. to “5. Repronicibility poor’. (3) Proper selection of wavelength. clogging Make sure the following points before starting checking. This applies also (1) Deterioration of lamp in the atomic absorption photometer. (2) Current level of hollow cathode lamp. (4) Alignment of absorption cell to optical axis. (5) Piping tube, joint and other parts involve none of leak, stale and Reagent staled. Replace reagent with new one. Absorption cell deteriorated. Replace absorption cell with new- cone. Standard service life is 50 hrs. Devitrfication reduces sensitivity. Flow rate of reagent and/ or sampl insufficient, (1) Pump speed too low. (2) Pump tube deteriorated. (3) Leak at piping system. (4) Pump tube compressed (at clamp). (5) Supply gas flow increased. Raise pump speed to proper flow- rate, Replace pump tube. Replace joint and tube. Remake sealing. Remove compression. Readjust or replace pressure regu- lator or needle valve.Troubles Causes Countermeasures 5. Reproducibility poor. ‘Sample flow rate improper. Readjust flow rate. Drain tube clogged to prevent flow| of waste solution. Let waste solution flow smoothly. Staled pump tube to cause inter- mittent aspiration Replace pump tube. (Standard service life 100 hrs or so.) Motor runs unsmoothly. Replace motor or control PAC. Manifold clogged. ‘Wash or replace manifold. Leaking at piping. Replace staled tube andjor joint with new one. Regulator and/or needle valve defective. Replace regulator andor needle valve.41 42 4. Procedures of Adjustment Tools and Materials Required for Adjustment Flowmeter assembly (775-07217) Pressure gauge Skg/cm?(200-93553-02) Argon gas Stop watch Volumetric cylinder 10m] Reagents Sodium borohydride solution (0.4% NaBH, + 0.5% NaOH) Hydrochloric acid (5M HCl) Sample Arsenic standard solution (10ppb) Distilled water Flow Path Adjustment 4.2.1 Argon Gas (supplying gas) Flow Adjustment Needle valve NV Pressure switch Pressure gage vt Q Pressure regulater ‘Ar 3.2kgflem? Solenoid valve | Needle valve NV2 > 500 mi 500 ml 500 ml CO) xt Mm Fig. 1 Argon gas flow path -“"Flow meter (1) Connect the pressure gauge (Skgf/em?) to a free port of the pressure regulator. (2) Run argon gas at 3.2 4 0.ikgf/em?. (3) Turn ON the power switch of the main unit. (4) Set knobs of needle valve (NV 1 and 2) to the mid-point by returning from a fully closed position by 4 tums. (5) Set pressure to 2.5kgf/cm? by tuming knob of the pressure regulator. -5-(6) Connect low meter to the needle valve (NV 1), and tum knob to set the flow rate to 32.5 + Iml/min. The flow rate is to be read at the center of float. (7) Connect the flow meter to the needle valve (NV 2) and set the flow rate to 32.5 Iml/min in the same way. (8) Make sure that the pressure gauge reads 2.5 +0. 1kef/em®. If not, repeat steps (5) through (7). (9) Remove the flow meter from the path. 4.2.2 Operation Check of Pressure Switch (1) Reduce Arsupply pressure slowly from 3.2kgf/cm? until PRESSURE lamp lights up and the pump motor stops, and read the pressure, Standard: 2.7 ~ 2.9kgf/em*. (2) Raise Arsupply pressure gradually until PRESSURE lamp goes out and the pump ‘motor starts running, and read the pressure. Standard: 2.7 ~ 2.9kefiem?. (3) Set Ar supply pressure to 3.2kgf/em?. (4) Make sure that the pressure gauge reads 2.5kgf/em?. (5) Disconnect Ar gas supply tube. (6) Remove the pressure gauge and fit up a plug (blind lid) and apply pipe sealant to threaded segment. (7) Tum OFF power switch of the main unit. 4.2.3 Flash Timer Setting Set the timer dial to 22.5 sec (0.5 sec). Press the flash button and measure the flash time with a stop watch. Make sure that the flash time is between 20 and 25 sec. 4.2.4 Performance Check See ‘2, Performance Check’’.5. Construction and Principle of Operation See ‘‘Section 3 Construction and Principle of Operation’’ in the Instruction Manual. 6. Reagent Preparation 6.1 Tools Required for Reagent Preparation fo (1) Pipette Iml 1 ~ (2) Pipette sml 1 (3) Pipette 10m1 1 (4) Volumetric flask 100ml 2 (5) Volumetric flask 500ml 1 (6) Volumetric cylinder 500ml 1 (1) Beaker 100ml 2 (8) Rubber ball for pipetter 1 (9) Digital balance 1 (10) Polyethylene tank 500ml 4 (to be increased if necessary) (or larger, if necessary) - 6.2 Stock Reagents G (1) Sodium borohydride (NaBH,) special grade (25gr bottle) (2) Sodium hydroxide (NaOH) special grade (500gr bottle) (3) Hydrochloric acid (HCl) special grade (500ml bottle) (4) Arsenic standard solution (As 1000ppm) standard solution for atomic absorption analysis (5) Distilled water 6.3 Reagents Required for Adjustment and Inspection and Their Volumes (1) NaBH, (0.4% NaBH, + 0.5% NaOH soln) 100mI/unit @) SMHCI 100ml/unit (3) As (10ppb) 100ml/unit Notes: 1) The volumes are those required for testing 2 absorption cells. ww 2) If an absorption cell alone is tested, the requirement for As (10ppb) is 50ml. -7-6.4. Preparation of Reagents 6.4.1 Arsenic Standard Solution (As 10ppb) (1) Take Iml of As 1000ppm standard solution by usinga Iml volumetric pipette into a 100ml volumetric flask. Add distilled water to 100ml, to make As 10ppm solution. ———> 10ppm (2) Take 10ml of As 10ppm solution prepared in (1) by using a 10ml volumetric pipette into a 100ml volumetric flask. Add distilled waterto 100ml, tomake As Ippm solution, ———> 1 ppm = 1000 ppb (3) For making 500m! of As 10ppb solution, take Sml of Ippm solution prepared in (2) by using a Sml volumetric pipette into a 500ml volumetric flask. Add distilled water to 500ml to make As 10ppb solution. 6.4.2 NaBH, Solution (500ml) (1) Weigh 2.5gr of NaOH on a balance and put it into a 100ml beaker together with about 100ml distilled water to dissolve, (2.54 0.05gr) (2) Put the solution into a 500ml volumetric flask. Wash the inner wall of the beaker with about 100ml of distilled water and addit into the 500ml volumetric flask, Shake the flask vigorously to dissolve completely. (3) Put2.0grNaBH, into a 100ml beaker, add about 100m distilled water to dissolve, pourit into the 500m volumetric flask mentioned in (2) andmix up. (2.0gr+.0.05gr) (4) Add distilled water to the volumetric flask mentioned in (2) up to 500ml 6.4.3 5M HCI; 500m! (1) Put 280m! distilled water into a 500m! volumetric cylinder. (2) Add 200ml hydrochloric acid to the 500m! volumetric cylinder mentioned in (1) to make the total volume 480ml. 6.5 Cautions for Using Reagents (1) Reagents are to be prepared immediately before starting adjustment and inspec- tion. (2) The service life of prepared solution is 2 days when kept in a refrigerator. (3) Never handle sodium hydroxide (NaOH), which is caustic, with naked hands. (4) Keep the container of sodium hydroxide tightly sealed, because if is hygroscopic. (5) Whenever skin or cloth comes in contact with any of reagent, wash it in running water immediately. (6) Throughout the course of the measurement, keep the duct fan running to exhaust. (7) Collect waste solution of sodium borohydride in its own reservoir, without being mixed with other waste. -8-7. Parts List Front Side ITEMNO.| PART NO. DESCRIPTION REMARKS, 1 2206-17123 Pressing Plate For Sample Tube 2 206-17124 Pressign Plate ForNaBH, & HOT 3 206-17118 | Roller Assy 4 072-60319-02 | Cramp, DKN-13SP 5 064-14116-03 | SW, M-2015J-2G Flush SW 064-14127-01__| Bezel, AT-207-W 6 (072-20903 Lamp, BNA-3 Clear Flush Monitor 7 (072-20923 Lamp, BNA-3 RED Pressure Monitor 8 064-14144-03 | SW, JWZ2120-0103 Power SW 9 206-17127 Screw 10 034-01056-01 | Spring, KCO70-100-0180 i 206-17126 PIN 12 037-30059-07 | Dumper TM.96-07Left Side ITEM NO. |. PART NO. DESCRIPTION REMARKS: 1 7206-18032 Tray Assy 2 206-60250-03 | Tube Vinyl 1 3 206-60259-04 | Tube Vinyl 2Back Side ITEM NO. | _ PART NO. DESCRIPTION REMARKS. 1 032-53739-11 | Gear Head, 2GB30K 2 200-84586-01 | Control Motor, 2U3RGB-A 3 200-76026-04 | Line Voltage Selector 4 200-81013-02 __| Line Filter, FN322 5 066-19466-01 | Timer, PM48A-100H-AC100 6 206-1712 Input Port Assy. ef. p13 7 206-1714 Needle valve Assy. 8 07201023 Fuse, 0.5A 100~ 117V 072-01660-06 | Fuse, 0.34 220 ~ 240V “ieLeft Side (Cover Opened) ITEMNO. | — PARTNO. DESCRIPTION REMARKS 1 200-82206-01 | Trans, 30VA 2 200-84586-02 | Control PAC SS21L -12-Right Side (Cover Opened) (Inport Assy. P/N206-17112) ITEM NO. | _ PART NO. DESCRIPTION REMARKS. 1 206-17113 Valve Assy. 2 040-72532 Regulator, B2019-C 3 200-77006-21__| SW, Pressure M4014 4 200-62033-01 | Coppler, 33PM -13-a 8. Electric Circuit DiagramLINE VOLTAGE SELECTOR MAGNETIC VALVE |,__240v y coset) {3220 co PRESSURE SW LINE FILTER tose ov P_black black 5 oll ___wov black ce] com aS atz204 + cE] No whit. white S ‘white [Timer IO, © Dye & (hala Ht al GUD = ey ’ MOTOR white [19 i Qe! white | 2 1 @ 7 }-—_—____uhiite 4 @) FLUSH LAMP -————— te POWER Eee ron PUSH, | fellow 3 | yettow sw Sw - : 0 - yeltow(] & 472. waa CET 2 PANEL ASSY ( 7206-18031) a biu 2 plue ro 20 brawn [oe "20ka 7 Durple 5 SPEED CONTROL VR| CONTROL PAC Fig. 8.1 Electric Circuit Diagram -15~16-"9. Flow Path DiagramNaBH, HCL SAMPLE 7 oy Wire mark | blue Reaction Coit As Wire mark Pump tube 080 Manifold yellow __————————" pump tube 30 40a 3 i 5 Gas/Liquid Separator fo cm eM! 20cm 60cm wo NV2 MV <— PR PS GAS IN Fig. 9.1 Flow Path Diagram -17~18-