MERCURY ANALYZER ACCESSORY FOR Z-2000 SERIES ATOMIC ABSORPTION SPECTROPHOTOMETER Please read through this manual carefully and keep it in a safe place. © Before using the instrument, read the safety HITACHIINSTRUCTION MANUAL MERCURY ANALYZER ACCESSORY FOR Z-2000 SERIES ATOMIC ABSORPTION SPECTROPHOTOMETER Hitachi High-Technologies Corporation ‘Comiiah © Hitachi High Technologies Corporation 2004, All ght reserved. Printedin Jepan, Part No. 740.9028 TS (HF-LT)PREFACE. ABOUT THIS MANUAL..... IMPORTANT .. ASAFETY suMMaRY. FOREWORD 1 2. INSTALLATION PREPARATION, CONTENTS 1 . . IMPORTANT-1 Product Warranty. . -IMPORTANT-1 Installation, Relocation and After-sale ‘Technical Service... IMPORTANT-3 Disposal of This Instrument. IMPORTANT-3 Other Precautions... . MPORTANT-3 Handling of Chemicals and Samples. MPORTANT-3 .. SAFETY-1 A Definition of Alert Symbol and Signal Word...... SAFETY-1 A, General Safety Guidelines sseue SAFETY-2 A Warning Indications in this Manual +. SAFETY-b Precautions on Correct Usage SAFETY-7 Electricity... - SAFETY-/ Exhaust and Ventilation, . SAFETY-7 Handling of Burner and Magnet .. SAFETY-8 Handling of Hollow Cathode Lamps . SAFETY-9 OREWORD-1 4 1.1. Place of Installation....... 1.1.1. Installation Table .. 1.1.2 Installation Site Conditions 1.2 Check of Standard Equipment. 4.3. Items for User to Prepare 1.4 Assembly of Control Unit.. 1.8 Tubing se 24 Reagents..... 2.2 Setting Up the Atomic Absorption Spectrophotometer. . 2.2.1 Preparation of Instrument... 2.2.2 Setting of Measurement Condit 2.3 Mounting and Adjustment of Hg Cell 2.4 Preparation of Reduction Vaporizer..3. MEASUREMENT... 0s - senvscansns . 3.1 Preparation of Working Curve... 3.1.1 Preparing Working Curve in OPEN Mode....3-1 3.1.2 Preparing Working Curve in CIRCULATE Mode... 3-3 3.2 Sample Measurement. 4, MAINTENANCE, 44 Maintenance 4.2 Replacement Parts vents oie444 1. INSTALLATION 1.4 Place of Installation 14 1.2 Installation Table Installation Site Conditions Place the mercury analyzer accessory in front of the atomic absorption epectrophotometer. If space is not available in front of the spectrophotometer, a separate table will have to be proparod. A table measuring at least GO cm wide by 50 om deep and able to bear a weight of 10 kg or more should be prepared. ns are basically the same as for the atomic absorption spectrophotometer. Some reagents used with the instrument or vapor emitted from it may be toxle or harmful. So be sure to prepare sufficient exhaust and ventilation facilities.4.2. Check of Standard Equipment 4.2. Check of Standard Equipment Check the delivered components and their quantity against the standard equipment list. If any parts are missing or damaged or if you have any question, contact our nearest sales or service representative, 1.3. Items for User to Prepare Prepare the items indicated below. For the reagent concentration and method of preparation, refer to section 2.1. * Various reagents needed * Standard solution + Pump (Displacement: 5 Limin or greater, motor output: 100 V, 10 W or more) Refer to the pump instruction manual for details. 1-214 1.4 Assembly of Control Unit Mount the washing bottle and dryer tube in the control unit as shown in Fig, 1-1. Refer to section 2.4 for the preparation of the dryer tube. Flowmeter 508-1533 Dryer tube 508-1333, Selector valve 508-1521 Washing bottle 508-1522 753066 Fig. 1-1. Control Unit1.5 Tubing 1.5 Tubing Armercury cell (PIN 180-0451) must be prepared on separate order. Cut the furnished tube to an appropriate length (preferably as short as possible) for the connection. A tubing diagram is given below. Pump, Mercury cell 3 Dryer tube : = x Selector westingTotle 4 vANe” Reason vessel Fig. 1-2. Tubing Diagram15 Figure 1-3 shows details of the tubing for the selector valve. To pump outiet To owmeter inet tote net [Rear view} y Align the marks and attach the lever. [Panel side] Fig. 1-3 Tubing of Selector Valve24 Reagents 4) 6) 24 2. PREPARATION Nitric acid (containing less than 0.0001 mg of mercury per liter of nitric acid) Sulfuric acid (containing less than 0.001 mg of mercury per liter of sulfuric acid) Potassium permanganate solution (5%) Dissolve 50 g of potassium permanganate in distilled water and adjust to a total volume of one liter. Then filter the solution, or put into the solution a gold wire that has been preliminarily red-heated and cooled, and stir it for one to two days. Potassium persulfate or ammonium persulfate solution (5%) Dissolve 50 g of potassium persulfate or ammonium persulfate in distilled water and adjust to a total volume of one liter. (The mercury content must be less than 0.001 mg per liter of the solution. If crystallization takes place, dissolve the crystallized components by heating before use for measurement.) Hydroxylamine chloride solution (10%) Dissolve 10 g of hydroxylamine chloride in distilled water and adjust to a total volume of 100 mL. Purify it hy using dithizone carbon tetrachloride (0.02%) to reduce the mercury content to below 0.001 mg per liter. Stannous chloride solution (10%) Add 60 ml of sulfuric acid (solution of sulfuric acid and distilled water mixed at a ratio of 1:20 by volume) to 10 g of stannous chloride (salt containing 2H20) and dissolve it by heating while stirring. After cooling the solution, add water {0 obtain a total volume of 100 mL. (The mercury content must be reduced to below 0.001 mg per liter of the solution by bubbling nitrogen gas as necessary. The solution can be stored for a week without alteration.)24 Reagents 7) 3) (9) (10) Magnesium perchlorate (granular reagent of high purity for analytical use) Concentrated mercury solution Dissolve 0.1354 g of mercuric chloride in 85 mL. of nitric acid (solution of nitric acid and distilled water at a ratio of 10:75 by volume) and adjust to a total volume of 100 mL. One mL of this solution contains 1 mg of mercury. The solution can be stored in a glass bottle for six months without alteration.) Intermediate standard mercury solution Add 1 mL of nitric acid to 5 mL of concentrated mercury solution prepared in step (8), and add distilled water to obtain a total volume of 500 mL. (One mL of this solution contains 0.01 mg of mercury. The solution can be stored in a glass bottle for one month without alteration.) Standard mercury solution Add 1 mL of nitric acid to S mL of the intermediate standard mercury solution prepared in step (9), and add distilled water to obtain a total volume of 500 mL. (One mL of this solution contains 0.0001 mg of mercury.)224 2.2. Setting Up the Atomic Absorption Spectrophotometer 2.2.1. Preparation of Instrument ‘The following description pertains to measurement with the Z-2000 series spectrophotometer. Set up the spectrophotometer according to the instruction manual provided with it. (1) Mounting of Hollow Cathode Lamp Mount the hollow cathode lamp for mercury. NOTE: Prior to handling hollow cathode lamps, read the cautionary instructions attached to them carefully (2) Preparation of Exhaust Duct Turn on power to the exhaust duct to run the blower. A WARNING Inhalation of a toxic gas may harm your health. If you inhale the vapor emitted from a sample, you may suffer inflammation of the respiratory system. Be sure to ventilate the room well by turning on the exhaust duct. (3) Turing on Power to Spectrophotometer and PC Turn on the power switch of the spectrophotometer main unit. Wait at least 15 seconds after tuming on the spectrophotometer power switch, then turn on the power switches of a personal computer and peripheral units connected to it such as a printer.2.2. Setting Up the Atomic Absorption Spoctrophotometer 2.2.2 Setting of (1) Set the measurement conditions as follows. Measurement Conditions ‘+ Instrument conditions Signal mode : BKG Corr. Measurement mode : Peak height Wavelength 2 253.7 nm Wavelenath setting method: Automatic Time constant + 0.28 Lamp current : 60mA © Analytical condition: Atomizer : Hg cell Flame type + None Delay time : 0s Measurement time: 206 + Working curve table Calculation mode : Working curve Order Linear (change If necessary) Number of STD: 3 (change if necessary) STD Replicate: 1 (change if necessary) (2) Check the analytical conditions. (3) Prepare for measurement. (Click the Ready button.)2.3 Mounting and Adjustment of Hg Cell Ay DANGER J cardiac pacemaker may become faulty dus to the strong magnetic field produced by the magnet. ‘person who utilizes @ pacemaker should not come within one meter of the instrument, or should avoid handling the instrument altogether. A CAUTION Be careful not to let your hands get attracted to the magnet. Do not bring metal objects that include iron, such as a screwdriver, near the magnet NOTE: The atomizer section utilizes a magnet. The strong magnetic field produced may cause damage to a watch or magnetic card and so on. Avoid bringing such objects near the magnet. (1) Attach the Hg cell onto the fur fumished screws, ied holder using the (2) Mount the Hg cell holder to the magnet. (3) Adjust the position of the Hg cell so that it won't interrupt the light beam, then tasten it to the magnet with the fumished screws. (To facilitate this adjustment, place a piece of white cardboard over the slit.)2.4 Proparation of Reduction Vaporizer 2.4 Preparation of Reduction Vaporizer (1) Pour 50 mL of potassium permanganate solution (5%) and ‘50 mL of sulfuric acid (1+4) into the washing bottle. (2) Pack the dryer tube with granular magnesium perchlorate (see Fig, 2-1). The tube should be packed just hefore starting analysis, and re-packed each time the reagent becomes ineffective (every 30 measurements or so). Granuier megnesium Rubber stopper Dryer tube perchlorate ‘Glass wool’ (about 0.5 9) Fig. 2-1 The Dryer Tube (3) Connect an empty and clean reaction vessel to the nozzle and set the selector valve to OPEN. Then operate the Pump for cleaning the interior of the flow path, (4) With the pump operating, set the flow rate to 1.5 Limin.344 3. MEASUREMENT The following description concerns measurement with the 2.2000 series spectrophotometer. 3.1 Preparation of Working Curve 3.4.1, Preparing Working Curve in OPEN Mode There are two measurement modes, OPEN and CIRCULATE, that are selectable with the selector valve. NOTE: A single measurement mode must be used for a series of measurements, (1) Measure out 0, § and 10 mL of the standard mercury solution into separate reaction vessels. Add distilled water to each solution to obtain a total volume of 200 mL and shake it well. After adding 10 mL of sulfuric acid and 5 mL of nitric acid, again shake the solution well. NOTES: 1. The standard mercury solution should be prepared on the day of measurement. 2. The standard mercury solution should be. stored in a glass container. Before using the glass container for storage. preliminarily fillit with a different standard mercury solution and leave it for a day or so. (2) Add 20 mL of potassium permanganate solution (5%) and leave the solution standing for about 10 minutes. (8) Add 10 mL of potassium or ammonium persulfate solution (6%), and then heat the reaction vessel in a water bath at about 95 °C for two hours (a hot plate may be used for heating). (4) Cool the solution to room temperature. Add 8 mL of hydroxylamine chloride solution (10%) and shake it well for reducing excessive ions of permanganate. (6) Execute Auto Zero on the spectrophotometer main unit a43.4. Proparation of Working Curve (6) With the pump stopped, set the selector valve to a position between OPEN and CIRCULATE. (7) Thirty seconds before proceeding to step (8), add distilled water so that the reaction vessel is filled up to a division line of 250 mL. (8) Add 10 mL of stannous chloride solution (10%) to the ‘solution prepared at step (7) and immediately connect the reaction vessel to the nozzle. (9) Vigorously shake the reaction vessel for about two minutes for mixing, then set the selector valve at OPEN. (10) Start measurement on the spectrophotometer main unit. (11) When “Under meaeurement ... data acquisition” appears on the status bar of the monitor window in the spectrophotometer application, start the pump. NOTE: Absorption signal is not recorded unless “Under measurement ... data acquisition" appears on the window. (12) The absorption signal is recorded, (13) After confirming the absorption peak has passed, discharge the solution from the reaction vessel and wash the interior of the veeeel with distilled water. (14) When absorbance has returned to "0", stop the pump,3.1.2. Preparing Working Curve in CIRCULATE Mode 312 (1) Measure out 0, 5 and 10 mL of the standard mercury solution into separate reaction vessels. Add distilled water to each solution to obtain a total volume of 200 mL and shake it well. After adding 10 mL. of sulfuric acid and § mL. of nitric acid, again shake the solution well NOTES: 1. The standard mercury solution should be Prepared on the day of measurement. 2. The standard mercury solution should be stored ina glass container. Before using the glass container for storage, preliminarily fill t with a different standard mercury solution and leave it for a day or so. (2) Add 20 mL of potassium permanganate solution (5%) and leave the solution standing for about 10 minutes, (3) Add 10 mL of potassium or ammonium persulfate solution (5%), and then heat the reaction vessel in a water bath at about 95 °C for two hours (a hot plate may be used for heating) (4) Cool the solution to room temperature, Add 8 mL of hydroxylamine chloride solution (10%) and shake it well for reducing excessive ions of permanganate. (8) Execute Auto Zero on the spectrophotometer main unit. (6) With the pump stopped, set the selector valve at CIRCULATE, (7) Thirty seconds before proceeding to step (8), add distilled waler so that the reaction vessel is filled up to a division line of 250 mL. (8) Add 10 mL of stannous chloride solution (10%) to the solution prepared at step (7) and immediately connect the reaction vessel to the nozzle, (9) Vigorously shake the reaction vessel for about two minutes for mixing. (10) Start measurement on the spectrophotometer main unit.3.1. Preparation of Working Curve (11) When “Under measurement ... data acquisition” appears on the status bar of the monitor window in the spectrophotometer application, start the pump. NOTE: Absorption signal is not recorded unless “Under measurement ... data acquisition” appears on the window. (12) The absorption signal is recorded. (13) After confirming the absorption peak has passed, set the selector valve at OPEN. (14) When the absorption decreases, discharge the solution from the reaction vessel and wash the interior of the vessel with distilled water. (15) When absorbance has returned to “0”, stop the pump.32 3.2. Sample Measurement (1) Collect sample in a glass or hard polyethylene vessel (preliminarily washed well with nitric acid and rinsed with water) NOTES: 1. A standard for the sample collection method is given in JIS KO094. 2. The sample stored in a glass vessel should be analyzed within a month after sampling, and that stored in a hard polyethylene vessel within two weeks after sampling. (2) Put 200 mL of sample into the reaction vessel. (Ifthe sample contains more than 0.002 mg of mercury, reduce sample volume by adding distilled water and bring the total volume to 200 mL.) (2) Add 10 mL of sulfuric acid and 5 mL of nitric acid to the sample and shake it well (4) Further add 20 mL of potassium permanganate solution (8%), shake well and leave It standing for about 15 minutes. If the crimson color of permanganate ions disappears, add potassium permanganate In increments of one gram so that the crimson color will last for 15 minutes. NOTE: When potassium permanganate is arded, calculate the blank value corresponding to the added amount for correcting the test result obtained. (5) Add 10 ii. of potassium or ammonium persulfate solution (5%), and then heat the reaction vessel in a water bath at about 95 °C for two hours (a hot plate may be used for heating) (6) Cool the sample to room temperature. Then add 8 mL of hydroxylamine chloride solution (10%) and shake it well for reducing excessive ions of permanganate,3.2 Sample Measurement (7) Execute Auto Zero on the spectrophotometer main unit. (8) Carty out measurement according to 3.1.4 (6) to (14) in the case of OPEN mode, or 3.1.2 (6) to (15) in the case of CIRCULATE mode.4.1 Maintenance (2) (3) 44 4. MAINTENANCE When the window of the Hg cell becomes soiled with fingerprints or dust, wipe it off with soft paper moistened with alcohol. When the interior of the Hg cell becomes contaminated, remove the holder and wash the interior with a chromic acid mixture. Then rinse with distilled water five times or so and with alcohol twice. Finally connect the cell to the suction side of the pump for drying ‘When the entire flow system is contaminated with mercury, fill the reaction vessel with 250 mL of ammonia water (1420). With the selector valve turned to CIRCULATE, Operate the pump for about § minutes. Then with the valve turned to OPEN, operate the pump for 30 minutes.42 Replacement Parts 4.2 Replacement Parts Following is a list of the part names and part numbers of the replacement parts. Part Name Part No. Remarks Reaction vessel 508-1330 Nozzle 508-1334 Dryer tube 508-1333 With rubber stopper and L-shaped pipe Selector valve ‘508-1521 Washing bottle 508-1522 Flowmeter 508-1533 Vinyihose 7x 10,10m__| F229009 Glass wool 1g 119021 Hose band 12, setofS | 1302016.05 Hg cell set 180-0451 Hg cel (cell alone) 180-4025INDEX A Ammonium persulfate solution. Analytical conditions ..., Atomizer . c CIRCULATE... Calculation mode. Concentrated mercury solution Control unit... D Data acquisition ... Delay time. Dryer tube... E Exhaust duct, 223 F Flame type... 24 H Hg cell. Holder Hollow cathode lamp. Hydroxylamine chloride solution. INDEX 4Installation... Installation site Installation table. Instrument conditions... Intermediate standard mercury solution Items for user to prepare. L Lamp current....... M Magnesium perchlorate .. Magnet...... Maintenance. Measurement. Measurement conditions. Measurement mode... Measurement time... N Nitric acid... 21 ,2-2,3-1,3-3,3-5 .3-1,3-2,3-4,3-6 Permanganate ions. svsnenes 25 Potassium permanganate 313-335 Potassium permanganate solution. 2-6,3-41,3-3,3-5 Potassium persulfate solution . 21 34,3-3,34 Pump 2,2-6,3-2,3-3,3-4 R Reduction vaporizer... Replacement parts... INDEX -2Ss Sample ss 0 35 Selector valve 1-9,1-4,1-5,2-6,3-4,3-2,3.3,34 Signal mode.... -4 Standard equipment. oo 12 Standard mercury solutior on 2-2,3-1,3-3 Stannous chloride solution 24,3-2,3-3 Sulfuric acid... 3-1,3-3,3-5 T Time constant 224 w Washing bottle. Wavelength Wavelength setting method. Working curve... Working curve table INDEX -3