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1.2  Theory of operation

750 Autosampler

3

Number of injections

The number of injections per sample with the 750 Autosampler de-

pends on the sample loop size. With sample loops > 10 

µ

L max. 3,

with sample loops 

 10 

µ

L max. 4 injections are possible. 

Fig. 3

 details

the needle position and displacement volume at the sample delivery

action. Care should always be taken that the injection volume is at least

three times greater than the volume of the sample loop. This is why only

a maximum of 2 injections per sample should be made with 100 

µ

L

loops; the minimum sample volume is 300 

µ

L for 1 and 600 

µ

L for 2 in-

jections. For sample loops with a volume 

 10 

µ

L up to 4 injections per

sample are possible. The minimum sample volume required is 150 

µ

L

for 1, 300 

µ

L for 2, 450 

µ

L for 3 and 600 

µ

L for 4 injections.

Rinsing

Rinsing will be necessary for highly concentrated samples or for sam-

ples that may absorb in the tubing or in the injection valve. Rinse vials

are filled with eluent or other suitable solvent. The Rinse process is

shown in 

Fig. 3

. Rinse vials can be used either after each vial (every

even numbered or odd numbered vial) or at programmed vial intervals.

There are two types of Rinses, the Normal Rinse and the Quick Rinse.

The 

Normal Rinse

 occurs after all the injections have been made from

the sample vial and the run time has elapsed. A 

Quick Rinse

 occurs

immediately after an injection and is used in applications where the

sample solution must not be left in the needle, transfer tubing or valve

for whatever reason. Only one injection per vial can be programmed

when using a Quick Rinse.

Injection

1 Injection

per vial

2 Injections

per vial

3 Injections

per vial

4 Injections

per vial

Rinse

1

2

3

4

2.65 cm
730

 

µL

1.63 cm
450

 

µL

1.02 cm
280

 

µL

1.63 cm
450

 

µL

0.51 cm
140

 

µL

0.51 cm
140

 

µL

1.12 cm
310

 

µL

0.51 cm
140

 

µL

0.51 cm
140

 

µL

0.51 cm
140

 

µL

2.65 cm
730

 

µL

 

Fig. 3:  Displacement volume versus needle position

Summary of Contents for 750 Autosampler

Page 1: ...9101 Herisau Switzerland Tel 41 71 353 85 85 Fax 41 71 353 89 01 Internet www metrohm ch E Mail info metrohm ch 750 Autosampler 2 750 0020 Instrument version 8 750 1023 Instructions for Use 23 02 2000...

Page 2: ...2 1 3 Location 9 2 2 Connection to IC system 10 2 2 1 750 Autosampler as Master 10 2 2 2 732 IC Detector as Master 11 2 2 3 Connection to 762 with IC Net 12 2 2 4 Tubing connection 14 2 3 Mains connec...

Page 3: ...erfaces 51 5 2 1 Contact closure strips 51 5 2 2 RS232 interface 53 5 3 Standard equipment 54 5 4 Optional accessories 55 5 5 Warranty and conformity 56 5 5 1 Warranty 56 5 5 2 EU Declaration of confo...

Page 4: ...s a ca pacity of up to 128 samples which are transferred automatically into the sample loop of the 733 IC Separation Center The 750 Autosampler performs up to four fixed loop injections per vial at us...

Page 5: ...the cap down into the vial The piston action of the cap pressurizes the sample and forces it up through the needle and the transfer tubing 8 8 that is connected to the needle From the transfer tubing...

Page 6: ...mples or for sam ples that may absorb in the tubing or in the injection valve Rinse vials are filled with eluent or other suitable solvent The Rinse process is shown in Fig 3 Rinse vials can be used e...

Page 7: ...1 Display LCD comprising 4 lines each of 20 characters 5 5 Transfer needle 2 2 Keypad with function numeric and cursor keys details see chap 3 1 2 6 6 Holder for transfer tubing 3 3 Sample rack 6 2041...

Page 8: ...control details see chap 5 2 1 13 13 Mains switch switch to switch the instrument on and off I ON 0 OFF 10 10 Contact closure strip for external control details see chap 5 2 1 14 14 Mains connection...

Page 9: ...f the instru ment The Instructions for Use are organized as follows Section 1 Introduction General description of instruments control parts and safety notes Section 2 Installation Installation of the...

Page 10: ...see Instructions for Use 762 READY SELECT A FUNCTION Display Text in display 1 1 of the 750 Auto sampler Hazard This symbol draws attention to a possible danger to life or of injury if the associated...

Page 11: ...s a danger of coming into contact with compo nents which are live Always disconnect the instrument from all voltage sources before you open it and ensure that the mains cable is disconnected from main...

Page 12: ...free transport of the instrument 2 1 2 Check After receipt immediately check whether the shipment is complete and has arrived without damage compare with delivery note and list of accessories in secti...

Page 13: ...strip 9 9 The four cable ends are appropriately inscribed with LOAD NO green LOAD COM yellow INJECT NO brown and INJECT COM white Connect the other end of the 6 2128 100 cable to the con nections Grou...

Page 14: ...atically stopped important for unattended continuous operation 1 Electrical connection 750 733 Connect 6 2140 020 connector plug to contact closure strip 9 9 and 6 2140 010 connector plug to contact c...

Page 15: ...operating the IC system with 732 IC Detector as Master 750 Autosampler Run Time 0 0 min 732 IC Detector operation with cycle program with command valve A B fill at time 0 0 min 2 2 3 Connection to 762...

Page 16: ...100 cable to the con nections Ground Fill and Inject on the terminal block 38 38 valve A or 46 46 valve B of the 733 IC Separation Center The three cable ends are appropriately inscribed with GND whi...

Page 17: ...6 and pull 6 1803 000 PTFE capillary tubing so far through the opening of holder stopper 7 7 that the tubing length between needle connection and the holder stopper is about 30 cm Then press holder st...

Page 18: ...ains cable Disconnect mains cable from mains connection plug 14 14 of the 750 Autosampler see Fig 5 2 Remove fuse cassette Using a screwdriver loosen fuse cassette 15 15 alongside the mains connection...

Page 19: ...g with an earthing pin If a different plug has to be fitted the yellow green lead IEC standard must be connected to protective earth protection class 1 Any break in the earthing inside or outside the...

Page 20: ...500 L of a suitable standard ion solution should be placed in position 1 of sample rack 3 3 then proceed step by step as follows 1 Switch on 750 Autosampler Switch on 750 Autosampler with mains switch...

Page 21: ...the SYSTEM key FUNCTION 4 The fol lowing screen will appear SYSTEM SETTINGS Park Needle Contact Closures Loop Size 7 Park needle Press the ENTER key The transfer needle will be withdrawn from the sam...

Page 22: ...ows the title of the selected function Parameters which can be edited with the numerical and or cursor keys are shown beneath If the arrows or appear at the right hand side this indi cates that the cu...

Page 23: ...or key to confirm the selection 3 1 2 Overview of key functions RINSE INJECTION MANUAL METHOD REM LOC TEMP SYSTEM F3 F2 F1 4 7 CLEAR 1 0 8 9 5 6 2 3 FUNCTION RUN STOP PRIORITY ENTER Fig 8 Keypad The...

Page 24: ...ry of number 7 Method Selection of method menu for editing or deleting methods INJECTION MANUAL 8 Numeric entry 8 Numeric entry of number 8 Manual injection Selection of the MANUAL INJECTION menu for...

Page 25: ...Shipping position Transfer needle is moved to the shipping position Point Entry of decimal point CLEAR Delete reset Deletion of an entered parameter and or resetting to default value Escape Exit from...

Page 26: ...tings show all dia log items which appear under SYSTEM The values shown in the displays are the default values the possible entry values or ranges are shown below the display SYSTEM SETTINGS Park Need...

Page 27: ...0 L Four injs vial 1 100 L Entry of loop size Entry of loop size in L In the bottom line the number of possible injections per sample is displayed For a volume of 10 L the maximum is 4 for a volume 10...

Page 28: ...Switching is made by means of the or cursor keys SYSTEM SETTINGS Time Date Date time settings By pressing ENTER the following screens are displayed Time Date 02 23 00 03 31 AM Display of date and time...

Page 29: ...INJECTION key FUNCTION 8 allows manual injections of a user specified sample When pressed the following screen is provided MANUAL INJECTION Sample Vial 1 Needle Depth POS 1 Run Injection Exit Manual...

Page 30: ...lowered to the selected position When the sam ple loop has been filled the injection valve is returned to the INJECT position The following display appears while the injec tion is being carried out au...

Page 31: ...of a menu point are accessed using the ENTER key and exited by pressing simultane ously the FUNCTION CLEAR keys The following listings show all dialog items which appear under METHOD The values shown...

Page 32: ...ample series defined in this program step If the numbers of the first and last samples are identi cal then this program step applies only to this single sample If the transfer needle is removed from t...

Page 33: ...selected which is longer than the run time METHOD N STEP M Event2 Time 0 0 0 0 999 9 min Time for event T2 Selects the time after which a signal in the form of a contact closure will be produced at o...

Page 34: ...s to whether a new program step is to be added ENTER Add a new program step CLEAR Return to program step menu METHOD N STEP M Previous Step Previous program step Changes to previous program step in th...

Page 35: ...1 10 Select method Entry of the method number N which is to be started After confirmation with ENTER the selected method is carried out exactly as if it has been started with the RUN STOP key details...

Page 36: ...the method number N which is to be deleted After confirmation with ENTER the following display appears Delete Method N ENTER to Delete CLEAR to Abort Confirmation of deletion process ENTER Delete sel...

Page 37: ...NN of current method STEP Number MM of program step METHTIME Total elapsed time since method start VIAL Number nnn of current vial INJ Number m of current injection RTIME Run time of current sample Wh...

Page 38: ...ons 1 Run Time 3 0 Event1 Time 0 0 Event2 Time 0 0 Event3 Time 0 0 Run Sample Exit Parameter menu for priority sample Number of sample vial for priority sample Number of injections 1 4 Run time Time f...

Page 39: ...isplays are the default values the possible entry values or ranges are shown below the display REMOTE LOCAL Local Switch to normal operation After confirmation of this command with ENTER the instrumen...

Page 40: ...e RS232 interface The value entered here must also be set on the external controller After the stop bits have been confirmed with ENTER the fol lowing display appears REMOTE MODE RS 232 Instrument in...

Page 41: ...ead vial number The position 1 128 HOME is put out Read injection valve position The position LOAD INJECT is put out Read x position The x position 0 760 is put out Read y position The y position 0 10...

Page 42: ...eedle into the vial displaces enough liquid to force the air completely through the injector valve loop and through the waste outlet tube Should any air remain in the vial it will be above the needle...

Page 43: ...s as this causes the filter to become blocked which also blocks the transfer needle Those samples which are difficult to filter manually with a mem brane filter see Fig 9 should be centrifuged before...

Page 44: ...y pressing RUN STOP and ENTER Park the transfer needle 5 5 by pressing SYSTEM and Park Needle Switch off instrument by means of mains switch 13 13 2 Remove old needle Hold connection screw 21 21 with...

Page 45: ...lso be formed by the precipitation of buffer salts in the IC system With buffered samples it is recommended that the sample loop feed is rinsed with a large volume of pure water after sample injection...

Page 46: ...and use a syringe to force solvent through to check for blockage There should be no diffi culty in forcing solvent freely through the tubing Force solvent through the transfer needle in the same fashi...

Page 47: ...ves the transfer needle is lim ited so as to prevent the vial from bursting under pressure in the event that a plug occurs in the transfer needle transfer tubing or injection valve If more pressure is...

Page 48: ...move 6 2128 100 con nection cable to the 733 IC Separation Center and operate the injection valve manually by means of the FILL and INJECT keys Please inform Metrohm service if the valve can only be r...

Page 49: ...jection A nee dle stall generally occurs if the transfer needle hits an obstruction when attempting to enter the vial An obstruction may be from the tray or sample vial being seated incorrectly or the...

Page 50: ...is unable to determine the coordinates of a vial location Inform the Metrohm service Needle Drive Motor Stalled RS 232 32 The motor drive for moving the transfer needle up and down is blocked Remove...

Page 51: ...liary output command request R 4 Request invalid because autosampler is busy performing an operation R 5 Invalid buzzer request R 6 Invalid command request Autosampler did not recognize command R 8 In...

Page 52: ...g Control elements Display LCD 4 lines each of 20 characters character height 4 mm Keypad Membrane keypad made of polyester with 20 keys Mains switch At rear of instrument Mains connection Voltage 100...

Page 53: ...romagnetic compatibility EMC Emitted interference Standards met EN 55011 class A Immunity to interference Standards met EN 50082 1 Ambient temperature Nominal operating range 5 45 C at 20 80 atmospher...

Page 54: ...nections is shown in Fig 13 The output signals are emitted as contact closures between two connections the input signals must be applied in the same way between two connections START output signal for...

Page 55: ...ng sig nal for the injection of a new sample A precondition for this is that the run time Run Time in the method has been set to 0 0 In this case the run time will be determined externally GND ground...

Page 56: ...e e g 6 2134 000 Metrohm cable 9 pol 9 pol Remote operation of the Autosampler is carried out with the ASCII commands described in chap 3 8 An example of the use of these commands in a RS232 control p...

Page 57: ...losure strip 10 10 1 6 2140 020 Connector plug With 8 connections plugs into contact closure strip 9 9 1 6 2621 020 Open end spanner 7 32 1 6 2742 010 Dust cover Dust cover for Autosampler 750 1 6 274...

Page 58: ...ting cable 750 709 length 2 m 6 2620 130 Transfer needle Replacement needle assembly see chap 4 2 2 6 2413 000 Borosilicate glass sample vials Set of 1000 with 1000 stoppers transparent and 100 stoppe...

Page 59: ...absence of guaranteed features the purchaser has no rights or claims except those mentioned above If damage of the packaging is evident on receipt of a consignment or if the goods show signs of trans...

Page 60: ...EWG Source of the specifications EN 50081 1 Electromagnetic compatibility basic specification Emitted Interference EN 50082 1 Electromagnetic compatibility basic specification Interference Immunity E...

Page 61: ...to the standards EN55011 class A EN50082 1 Electromagnetic compatibility IEC1010 EN61010 UL3101 1 Security specifications It has also been certified by the Swiss Electrotechnical Association SEV which...

Page 62: ...claration of conformity 57 Delete 22 Delete a method 33 Delete Method 33 Delete program step 32 Delete Step 32 Depth 24 50 Dimensions 50 Displacement principle 2 Displacement volumes 3 24 27 Display 1...

Page 63: ...igure 42 Replace transfer needle 41 Needle position 3 Needle settings 24 Needle Setup 24 Next program step 31 Next Step 31 NO 23 Non reproducible injections 43 Normal closed 23 Normal open 23 Normal o...

Page 64: ...rce method 32 Standard chromatogram 17 Standard equipment 54 Start Vial 29 Static charges 8 Status 25 Status display 25 Status display for method 34 Status display for priority sample 35 Steel capilla...

Page 65: ...5 Appendix 750 Autosampler 62...

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