SECTION J Drug Chemistry Section Drug Chemistry Procedure
Contents
1. Drug Chemistry Section Modification of J 3 Drug Chemistry Procedure Manual Prepared by R W Waggoner Jr Effective Date March 15 2003 Approved by D J Koontz Supercedes September 1 1996 Name of Procedure Toxicology Use of the Hamilton Microlab 1000 plus and Microlab 500 Liquid Handling Systems to Prepare Samples Suggested Uses This procedure is designed to prepare most liquid samples for the analysis of some volatile substances specifically low boiling point alcohols by gas chromatography with headspace sampling The Hamilton Microlab instruments may also be used for other sampling when necessary The use of an internal standard in gas chromatography can be done by delivering accurate amounts of the sample to be analyzed and of an internal standard The use of an automated system for measuring and delivering liquids is comparable if not better in precision and accuracy to manual methods The Hamilton Microlab 1000 plus and Microlab 500 liquid handling systems improve speed and accuracy of preparing samples for analysis of volatile substances using headspace gas chromatography methods Apparatus Needed to Perform Procedure Hamilton Microlab 1000 plus or Microlab 500 liquid handling system Headspace sample vials Magnetic seals Hand crimper Liquid waste container suggested 250 mL beaker Kimwipes or equivalent Volumetric flask Reservoir for the diluent solution Deionized water Quality Control The Quali2. eparation using the Microlab 1000 plus a b The following steps can be activated by two ways press the ENT key or press the button on the wand The sample to be analyzed is collected by placing the tubing on the right side of the system into the sample and aspirating the sample by pressing the button The outside of the tubing is wiped with a clean Kimwipe or equivalent to remove excess sample residue The sample diluent are dispensed into the proper vial by pressing the button again The tubing is washed between each sample by aspirating an air sample and then dispensing the air diluent into a waste container The washing procedure flushes the sample tubing with 1 8 mL of diluent The sample tube is then wiped again and the next sample is ready to be collected Seal the vials place the seal on top of the headspace vial and crimp the seal with the hand crimper The seal should not be loose enough to remove by hand 2 Sample preparation using the Microlab 500 The following steps can be activated by two ways press the Run Stop key or press the button on the wand Allow the left syringe to fill and the air gap on the right syringe to fill The sample to be analyzed is collected by placing the tubing on the right side of the system into the sample and aspirating the sample by pressing the button The outside of the tubing is wiped with a clean Kimwipe or equivalent to remove excess sample residue The sample d
3. iluent are dispensed into the proper vial by pressing the button again Seal the vials place the seal on top of the headspace vial and crimp the seal with the hand crimper The seal should not be loose enough to remove by hand Allow the left syringe to fill and the air gap on the right syringe to fill before proceeding to the next sample The tubing is washed between each sample by aspirating an air sample and then dispensing the air n propanol into a waste container The washing procedure flushes the sample tubing with 1 8 ml of diluent Maintenance 1 The tubing should be flushed with a Clorox solution or equivalent about once every few months to remove protein build up and prevent bacterial growth in the tubing Comments 1 The liquids being sampled should be warmed to room temperature before use 2 Any liquids containing volatile substances should be covered or sealed to prevent evaporation of the volatiles The reservoir containing the diluent solution should be closed but not sealed to prevent a vacuum from forming in the reservoir Safety Concerns When working with biohazardous samples use protective measures such as gloves laboratory coat eye protection and work with the samples in a biosafety hood Literature References Hamilton Microlab 1000 plus User Manual part number 610 370 01 Hamilton User s Manual Microlab 500 B C Series part number 69176 Rev B
4. tinue J 3 Hamilton Microlab 500 Start up a Turn power on Switch is on the front of the unit at the bottom right Selections on the display screen can be entered by pressing the Run Stop key The arrow keys can be used to move from one data entry field to another Values can be entered via the numeric keypad Microlab 500 program If program has been entered skip this step note entries to be selected are in bold face type a b Main Menu Create a new Method or Edit an existing Method Select Select Method Name Select Method Title Ratio 1 9 0 Dilution 1 10 0 Left Diluent Volume uL 1800 0 Right Air gap volume uL 10 0 Right Sample volume uL 200 0 Final Volume uL 2000 0 ACCEPT when complete Syringe Fill speed Left 3 Syringe Aspirate speed Right 1 Syringe dispense speed Left 3 Right 2 Syringe Fill mode AUTO Air gap mode AUTO air gap delay 0 0 ACCEPT when complete Wash volume uL 0 0 Left syringe fill speed 4 Left syringe dispense speed 4 ACCEPT when complete CONFIRM to Save Method ESCAPE to cancel 3 Running the Method oao From the main menu select Run an existing method Highlight the appropriate method and press SELECT Left syringe size uL 2500 0 Right syringe size uL 250 0 CONFIRM The system will purge g Place the left diluent tube in the diluent solution and prime the system Application of Procedure on Evidence 1 Sample pr
5. ty Control of the system is verified by use of known standards each time the system is utilized SECTION J Instrument Set Up for blood alcohol analyses A Hamilton Microlab 1000 Plus 1 Start up a Turn power on Switch is on the back of the unit at the bottom right Selections on the display screen can be entered by pressing the ENT JA YES key Different selections can be displayed or highlighted by pressing the NEIN NO key Values can be entered via the numeric keyboard 2 Microlab 1000 plus program If program has been entered skip this step note entries to be selected are in bold face type a b C 2ogp Method enter method Function Dil Diluter Vol Air gap 10 ul Asp Automatic Air yes Sample Vol 200 ul Diluent ul Diluent 1800 ul Wash Vol 0 ul Wash Step 1 Syr A Syringe AD 2 5 ml B Syringe DAD 250 ul Standard tubing yes Speed these are only suggested values Asp sample 2 sec Disp sample 2 sec Asp diluent 4 sec Disp diluent 3 sec Running the method Select and enter RUN Choose method containing program Press enter to zero the syringes Place the diluent tubing on the left of the Microlab 1000 plus into the diluent solution Prime the system by pressing the ENT key at the prompt PRIME The system should be primed five times before use to clear the tubing of air and any residue Once priming is done press the NO key to con
Download Pdf Manuals
Related Search