SOP for Operation of Atomic Absorption Spectrometer with graphite furnace.

1.0    Objective:

               To provide written procedure for operation of Atomic Absorption Spectrometer with graphite furnace.

2.0       Scope:          

            This SOP covers operation of Atomic Absorption Spectrometer with graphite furnace;

Make - Varian.

3.0       Responsibility:

            Jr. Research Officer, Research Officer: Responsible for operation, calibration and maintenance of the instrument as per procedure.

            Head of Department: Responsible for calibration and maintenance, timely as per schedule.

            QA Officer/QA Manager: Review the records and governing the document.

4.0       Procedure:

4.1       Ensure that the instrument is clean and free from dust.

4.2       Operating Procedure:

4.2.1    Open the outlet of the Nitrogen cylinder supply.

4.2.2    Switch ‘ON’ the cold-water pump, which is required to control the temperature in graphite furnace. The water flow must be more than 1.5 to 2.0 liters per minutes with pressure.

4.2.3 Switch ‘ON’ the computer system, monitor and the instrument.

4.2.4  Programmable sample dispenser (PSD) is attached on the front side of instrument. 

4.2.5 Keep the standard vial and sample vial in PSD at their respective position.

4.2.6    Double click on the spectrAA icon.

4.2.7   Click on Worksheet icon, open new worksheet then give the name of worksheet, adds the number of sample to run and click ok.

4.2.8   Click on ‘add method’ icon and select the method. Place a Hollow Cathode Lamp as per selected method in a lamp holder positioned to the right of the instrument.

4.2.9    Click on ‘Edit method’ icon and open the dialogue box.  

4.2.10  Select Automix or Premix in Sampling mode, select peak height in measure mode, select concentration in calibration mode, select the lamp position and background correction in optical mode, fill respective standard concentration then keep vial in their respective place and adjust the volume of the blank & bulk which is to be adjusted in the sampler mode.  If modifier is used, place the modifier in their respective position and update their position in the sampler mode & click OK.

4.2.11    Click on ‘Labels’ icon and name the labels, write the sample weight and sample volume   before analysis.

4.2.12    Click on ‘instrument’ icon then click on optimize icon, select method and click OK.

4.2.13    For furnace facility press shift +F7 key and align the tube. After proper alignment of tube close the furnace facility.

4.3            Programmable Sample Dispenser:

4.3.1        In Carousel 1 to 45 number are for sample vial, 46 to 50 number for premixed standard,

            52 number for blank vial and 53 to 55 for modifier.

4.4       Setting up the Capillary:

4.4.1        A mirror is used to see inside the graphite tube to check the alignment.

4.4.2        Capillary is correctly located in the vials when picking up sol.

4.4.3        The capillary should enter or leaves in the graphite tube atomizer without touching the sides of the injection hole.

4.5              Graphite Tube Atomizer:

4.5.1    Place the partition graphite tube by opening the burner shield & place the tube in such a

            manner that the hole of the tube should be positioned towards the rear of the right-hand

side of the burner shield.

4.5.2        The liquid trap attached at the bottom of the PSD should be filled with D.D. Water.

4.6       Report:

4.6.1        Double click on the SpectraAA icon, click on ‘report’ icon. Select the worksheet. Then click next for two times select the sol. data, report contents. In report contents only select the standards & also select the calibration graph report.

4.6.2        Then click next the report is generated to see the report click on print preview or print out the report click print report.

4.7              After completion exit the soft ware & switch off the instrument.

4.8              Record the usage of instrument in usage log book of instrument.

5.0      Precaution:

5.1       Do not touch the quartz lamp envelop with bare hands. Skin oils may be absorbed into the

quartz. Always use clean cotton gloves when handling lamps. If contact is made with the lamp surface, clean immediately with propanol.

5.2         The liquid trap must be filled with the same solvent as that used for the analysis.

5.3        Ventilate the working area by using an efficient extraction system to remove burnt gases.

6.0         Calibration:

Check the performance of the instrument quarterly

7.0        Maintenance:

7.1       Clean the instrument with wet cloth than dry.

7.2       Replace the water in liquid trap.

8.0       Documentation:

            Annexure – 1    Instrument Usage logbook              XXX/FRM/000

9.0       History of Revision:

Revision No.	Effective Date	Revision details	Reason for revision

Annexure - 1
Date	Name of Sample	A. R. No.	Batch No.	Analyzed by	Remarks
SOP No. : XXX/SOP/000 -00                                      Format No. : XXX/FRM/000-00