Allied Telesis 6870 User Manual

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15 Liberty St., Metuchen NJ 08840 1-800-LAB-SPEX(1-800-522-7739)ext 465

6870 FREEZER/MILL®

OPERATING MANUAL

This manual is part number 85018

 

TABLE OF CONTENTS

 

SECTION

DESCRIPTION

PAGE

1.0

Introduction..................................................................................................................................

3

2.0

Specifications...............................................................................................................................

4

3.0

Unpacking....................................................................................................................................

5

4.0

Setting Up ....................................................................................................................................

6

5.0

Touch Screen Displays................................................................................................................

9

6.0

Practical Operation ....................................................................................................................

14

 

6.1 Adding Liquid Nitrogen Coolant…………………………………………………….14

 

6.2 Loading Samples into Freezer/Mill Vials……………………………………………15

 

6.3 Removing, Opening, Emptying, and Cleaning Freezer/Mill Vials…………………..17

 

6.4 Checking Liquid Nitrogen Level…………………………………………………….20

 

6.5 6820 Auto-FillSystem………………………………………………………………20

 

6.6 6814 AutoExtractor………………………………………………………………….21

 

6.7 Maintenance…………………………………………………………………………21

7.0

Warranty and Service ................................................................................................................

21

8.0

Trouble-ShootingGuide............................................................................................................

23

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SECTION 1.0: INTRODUCTION

SPEX SamplePrep Freezer/Mills are cryogenic laboratory mills that cool samples to cryogenic temperatures, and pulverize them by magnetically shuttling a steel impactor back and forth against two stationary end plugs. Since the vial is closed, the integrity of its contents is maintained: hazardous or critical samples are easily controlled, cleanup is simplified, and crosssample contamination is eliminated. Because the vial is immersed in liquid nitrogen throughout the grinding cycle, the sample is kept at cryogenic temperatures and its key aspects preserved. These features have made SPEX SamplePrep Freezer/Mills the most effective cryogenic mills in the world. They are the “mills of last resort” for many normally ungrindable samples, or samples whose composition or structure is altered by the heat generated by conventional grinding.

Before operating the 6870 Freezer/Mill, familiarize yourself with these instructions. The Freezer/Mill is different in its principles and operation from any other laboratory mill. If you’re familiar with the mill and want to proceed directly to grinding, Section 6.0 (PRACTICAL OPERATION) on p.14 can serve as a general review of the actual operation of the mill. We suggest unpacking the mill, then going over its various features with these instructions in hand before attempting to add liquid nitrogen or grind a sample.

OPERATING CONDITIONS: Do not set up the 6870 Freezer/Mill in an insulated or confined space. The Freezer/Mill should be run on an open countertop, in ambient air. If the entire mill is chilled during operation, components like the gas cylinders can fail. This damage is not covered by the Freezer/Mill warranty.

VERY IMPORTANT: Liquid nitrogen not only makes samples brittle through severe chilling, making them “grindable,” but also cools the magnetic coil which powers the 6870 Freezer/Mill. If the mill is operated without liquid nitrogen for a period of about one minute, the coil will become very hot and may sustain permanent damage. The 6870 Freezer/Mill has a liquid nitrogen sensor that should shut down the mill when the liquid nitrogen gets too low to cool the coil. Nevertheless the nitrogen level should be visually checked during extended runs as well as topped off before every run. The Freezer/Mill warranty does not cover damage to the coil caused by operating the mill with little or no liquid nitrogen.

SAFETY NOTES:

1)Liquid Nitrogen can be hazardous. Its boiling point is -195.8o C. When working with liquid nitrogen directly or indirectly, you must wear cryogenic gloves to protect your hands. Be careful not to splash liquid nitrogen on clothes or unprotected skin. Always use cryogenic gloves when handling very cold objects or materials: sample vials, the nitrogen tank valve or hose, chilled Freezer/Mill components, etc. We also recommend safety goggles to protect your eyes.

2)Do not attempt to operate the 6870 Freezer/Mill without liquid nitrogen

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SECTION 2.0: 6870 FREEZER/MILL SPECIFICATIONS

Type of mill: cryogenic impact mill

Grinding mechanism: steel impactor driven by dual electromagnets Coolant: liquid nitrogen

Weight (empty, without vial or coolant): approx. 44 lbs. (20 Kg)

Grinding Vials: one 6801 Large Vial, one Mid-SizeVial (6871, 6881, 6885), or one 6753 Microvial set, also one to four Small Vials (6751, 6751/52, 6761, 6771).

Typical Sample Capacity:

Small Vials: actual volume with impactor, approx. 25 ml. Typical sample weights: 2 grams for biological samples, 1 gram for polymers. Effective capacity for a given sample is determined by trials. Overfilling a vial greatly reduces its efficiency. 6753 Microvial Set: 100 - 500 mg per individual 6753V Microvial, depending on sample.

Mid-SizeVials have up to 5 times the sample capacity of Small Vials, and Large Vials about twice the sample capacity ofMid-SizeVials.

Actual performance of any vial/sample combination depends on sample properties, cooling time, grinding time, desired outcome, etc.

Typical liquid nitrogen consumption:

10-15liters for initialcool-downand filling of the tub.4-6liters for each hour of operation

Actual LN consumption can vary.

Electrical specifications: CE Approved, available in 115V 60HZ or 230V 50HZ. Cord: 115V 60HZ version,3-pronggrounded plug supplied.

230V 50HZ version, 2-prongEuropean plug supplied.

Operator is responsible for supplying alternate line cord/plug if required.

Fuses: Two5-ampslow-blowfuses in AC Input module.25-ampslow-blowfuse on driver board

Dimensions: 20½ in. (52 cm) x 21½ in. (55 cm) x 18 in. (46 cm)

CE Compliance and Certification: The 6870 Freezer/Mill has been tested for compliance with CE Directives for Industrial, Scientific, and Medical Equipment Emission, and Generic Light Industrial Immunity.

Safety Features:

Lid Interlock prevents mill from running if lid is not latched shut. Liquid nitrogen sensor shuts down mill if liquid nitrogen level is too low.

NOTE: Liquid nitrogen level should be visually checked during extended runs as well as before every run. The Freezer/Mill warranty does not cover damage to the coil caused by operating the mill with little or no liquid nitrogen.

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SECTION 3.0: UNPACKING

Inspect the exterior of the packing box and report any visible damage to the carrier. Remove all packing documents from the exterior of the box, and save them for your records. Open the top of the shipping box. Remove the packing material and accessories, and gently remove the Freezer/Mill. Visually check the mill for any damage that may have occurred during shipping. Unlatch the lid and inspect the interior of the tub, ensuring that it is free of any packing material. Check the packing list to see that there are no parts missing, and inspect the accessories. If everything seems to be in proper order, we recommend you store the packaging materials, in case there you ever need to return the unit for warranty service or repair.

Grinding vials must be purchased separately and are available in three sizes: large, mid-size,and small. Each new 6870 Freezer/Mill includes an Acccessory Package to match your choice of vials, either the 6870L for large vials or the 6870S for small vials. Both include an extractor for removing end plugs from cold vials, and a vial rack; the 6870S also includes an adapter for running up to four vials in the 6870. A 6870M Accessory Package is available formid-sizevials, but must be used in conjunction with the 6870L. The full range of grinding vials and accessories for the 6870 Freezer/Mill is described in our catalog (Handbook of Sample Preparation and Handling) and on our website (www.spexcsp.com).

6870 FREEZER/MILL, FRONT VIEW

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6870 FREEZER/MILL, BACK VIEW

SECTION 4: SETTING UP

The 6870 Freezer/Mill weighs 44 pounds (20 Kg) empty. The lid opens from the front and the lid latch is in the center. The AC Input module is on the back of the cabinet, and includes the power switch and fuse tray. The fuse tray can be opened with small screwdriver or knife-blade.Also on the back of the cabinet is the vent from the liquid nitrogen tub. There are gas cylinders on both sides of the cabinet to control the movement of the lid. The control panel is on top of the lid, and can be detached for remote operation. It is connected to the lid by an RJ45 (“Ethernet”) cord. On the back of the lid is a USB port to let you link the 6870 Freezer/Mill to a PC or LIMS system.

4.1 Electrical Hookup

Plug the electrical cord into the inlet on the back of the Freezer/Mill cabinet, and then into a standard 3-pronggrounded electrical outlet. We recommend a fused20-ampcircuit for the 115V/60 HZ version. If you have the 230V/50HZ version of the mill, make sure the cord and plug conform to local electrical codes; we furnish the 230V/50HZ 6750 Freezer/Mill with a standard European2-prongplug with cord.

4.2 Power Switch and Control Panel

Electric power to the Freezer/Mill is controlled by the rocker switch on the inlet module. It is marked with two numerical symbols, zero (0) for “off” and one (I) for “on.” Press the one (I) side of the switch to turn the power on, or press the zero (0) side of the switch to turn the power off. When power to the mill is on, the control panel display will light up.

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The control panel is a touch-screen,activated by a stylus. The Freezer/Mill is programmed and operated through this control panel, whose successive screens are described and illustrated in Section 5, starting on page 8. Programmable parameters includepre-coolingtime, grinding time, cooling time between grinding periods, the number of grinding periods, and the rate of grinding. The control display also warns if the lid is not fully closed, or if there is not enough liquid nitrogen in the tub.

4.3 Lid and Lid Latch, Coil Assembly and Coil Gate, LN Sensor

The lid of the 6870 Freezer/Mill supports the coil (dual electromagnet assembly) and coil housing. To open the lid, hold the lid down with one hand, and with the other pull the upper end of the latch toward you. The lower end of the latch should disengage from the cabinet. Release the lid and it should be pushed up by the gas cylinders, which also keep the lid raised when open. The lid must be open to put vials in the coil and take them out. Liquid nitrogen (LN) is added with the lid open, unless the 6870 is equipped with the 6820 Auto-FillSystem.

The lid must be shut and latched for the Freezer/Mill to run. Push the lid down, hold it down while engaging the latch, then lock the latch by pushing its top end toward the cabinet.

The circular hole on the right side of the coil housing is where to insert a vial for grinding. The coil gate keeps the vial or vials in place during grinding, but must be lowered to insert or remove vials. The rectangular space toward the top of the coil housing is for pre-coolingloaded vials. (Do not run the 6870 Freezer/Mill without a loaded vial in the coil.)

The coil gate holds the vial or vials in the coil during grinding. To lock a vial in place, loosen (unscrew) the coil gate handle a turn or two, and position it so the handle passes through the slot in the coil gate when the gate is raised. Tighten the coil gate handle against the gate, so the gate contacts the vial snugly, but do not overtighten the gate as this can crack the plastic center section of the vial. When the coil gate handle is properly tightened, fold it down to lock the gate during grinding. Always use the proper Adapters forMid-Sizeand Small vials (see 4.4), andalways wear gloves when touching a chilled vial or any part of the chilled coil housing!

The LN sensor is behind a shield on the back wall of the LN tub. If there is not enough liquid nitrogen in the tub to start the mill, when RUN is touched the STATUS screen (p. 10) will display STATUS: LOW LN LEVEL. If the LN runs low during a grinding program the same message will appear and the program will stop. To continue running, fill the tub with liquid nitrogen to the mark. When RUN is pressed, the grinding program will start over.

To keep a run from being interrupted by the liquid nitrogen (LN) sensor, the LN level should be visually checked from time to time during extended runs, as well as before every run. The 6870 Freezer/Mill can run low on LN during extended runs, so should be checked after each 30 minutes of grinding time, and the LN topped off if necessary. The Freezer/Mill warranty does not cover damage to the coil caused by operating the mill with little or no liquid nitrogen.

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4.4 Grinding Vial Sizes, Adapters, and Vial Openers.

Large vials (6801, 6871) are run one at a time in the 6870 Freezer/Mill, without any adapter. Large vials are opened by the 6804 Extractor/Vial Opener, which is part of the 6870L Accessory Package.

Mid-Sizevials (6881, 6883, 6885) are run one at a time, but the 6886Mid-SizeAdapter must be placed in the coil first, to center and align anyMid-Sizevial.Mid-Sizevials can be opened by the 6804 Extractor/Vial Opener, but only by installing the 6884Mid-SizeVial Adapter for the 6804. The 6884 and 6886 Adapters comprise the 6870M Accessory Package.

Most Small vials (6751, 6761, 6771) can be run one, two, three, or four at a time in the 6870 Freezer/Mill. However, they must be used in conjunction with the 6806 Multi-VialAdapter, anX-shapedinsert for the coil. The 6806 Adapter keeps the vials parallel to each other and the coil, so each impactor moves back and forth in line with the magnetic field. Also, if a small vial were to be positioned diagonally inside the coil, the gate could not be properly tightened against the vial, and an end plug might work its way out of the vial during grinding. When running Small vials, make sure the coil gate contacts the end plug of every vial. If the gate needs adjustment to do this, the bottom or pivot end of the gate can be moved toward or away from the coil housing by turning the gate clockwise or counterclockwise on its mounting bolt.

Unlike other Small vials, the 6753 Microvial Set is run one at a time with the 6806 Adapter. Each 6753 set includes three 6753V Microvials. If more than one 6753 Microvial Set is placed in a 6870 Freezer/Mill, some of the individual Microvials will be shielded from the magnetic field, and grinding in those vials can be ineffective.

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SECTION 5.0: TOUCHSCREEN DISPLAYS

The 6870 Freezer/Mill is programmed and operated through a series of touchscreen displays. Transition between screens, and all programming and operating commands, are done by touching the screen with a stylus. Do not use a sharp point as this can damage or deface the screen.

5.1 LOGO SCREEN

When you switch on the power, the LOGO screen appears first. This says “SPEX SamplePrep 6870 Freezer/Mill” and includes a graphic representation of the Freezer/Mill mascot. Touch theLOGO screen anywhere to transfer to theCURRENT SETTINGS screen.

5.2 CURRENT SETTINGS SCREEN

This screen displays whatever program is currently set up to run. Here is a typical program, as displayed:

CYCLES

3

PRECOOL

10 MIN

RUN TIME

2 MIN

COOL TIME

2 MIN

RATE

10 CPS

SETTINGS

Start SCRN

CURRENT SETTINGS SCREEN

If the Freezer/Mill has a loaded vial in the coil, is filled with LN, and the lid is down and latched, this is what happens when the mill is started with these settings:

1)Precool: the coil is inactive while the vial cools under LN for 10 minutes.

2)First cycle: the coil is activated and the impactor grinds for 2 minutes at a rate of 10 cycles per second (20 impacts per second).

3)Cool time: the coil is inactive for 2 minutes while it and the sample cool back down.

4)Second cycle: the coil is activated and the sample is ground for another 2 minutes.

5)Cool time: the coil is inactive for 2 minutes.

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6)Third cycle: the coil is activated for the final 2-minutecycle. When it is done, the program is over and the sample has been ground for a total of 6 minutes.

5.3STATUS SCREEN

To run the program displayed on the CURRENT SETTINGS screen, touch “Start SCRN.” This transfers you to theSTATUS screen, which allows you to start the mill, stop it, or pause in the middle of a grinding program. (To change the settings, touch RTN on theSTATUS screen to go to theCURRENT SETTINGS screen. Touch SETTINGS to go to theSETTINGS screen, and see Section 5.4 for instructions.)

In the STATUS screen, the STATUS line displays the stage of the program: in a typical program, the sequence is STATUS: PRECOOL, STATUS: GRINDING, STATUS: COOL DOWN, STATUS: GRINDING, etc., to the end of the program, which is displayed as STATUS: RUN COMPLETE. Before a run this screen displays STATUS: STANDBY.

STATUS: STANDBY

Time Remaining: 0:00

Cycles Remaining: 0

RATE: 10 -----------

I -------

 

 

 

 

PAUSE

RUN

STOP

RTN

STATUS SCREEN before a run

To start the Freezer/Mill, press RUN. Before you do this, fill the tub with liquid nitrogen, place a loaded vial in the coil, and latch down the lid.

If there is not enough liquid nitrogen (LN) in the mill, the STATUS line of the STATUS screen will display STATUS: LOW LN LEVEL.

If the lid is not down and latched, the STATUS line will display STATUS: LID UP.

If the mill is filled with LN, and the lid is latched down, the STATUS line will initially display STATUS: INITIALIZING, then STATUS: PRECOOL. That marks the beginning of the grinding program.

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