Packing Procedure for 4 to 7.5 mm Liquid Samples. Sample Volumes of 46 to 450 µl Pub. No , Rev. C 0907

Transcription

1 Packing Procedure for 4 to 7.5 mm Liquid Samples Sample Volumes of 46 to 450 µl Pub. No , Rev. C 0907

2 Pub. No , Rev. C 0907 Packing Procedure for 4 to 7.5 mm Liquid Samples Sample Volumes of 46 to 450 µl Safety Precautions, page 2 Sizes and Sample Volumes, page 3 Sample Holder Parts and Tools, page 3 Packing the Sample, page 4 Removing the Liquid Sample, page C 0907 Sample Packing Procedure 1

3 Safety Precautions WARNING: Personal injury is possible if a spinning rotor explodes. Avoid eye and body injury from an exploding rotor by not spinning rotors outside magnet. Use a certified safety shield, full face shield, and cover all exposed skin at all times if it is necessary to spin a rotor outside the magnet. WARNING: explosions and potential injury are possible if rotors are spun beyond their maximum spin speed. Decrease the maximum spin rate by 20% if the sample density is above 6.0 g/cc. CAUTION: Do not exceed the sample VT range or spinning speed. Exceeding the sample VT range or spinning speed can result in failure causing damage to the rotor housing and or the probe. Liquids sample s have a specific VT and spinning speed ranges that may be different than the probe VT and spinning speed ranges. Refer to the documentation supplied with the sampler kit or contact Varian Technical Assistance and request the temperature and spinning speed ranges of the sample. A specification document is provided. CAUTION: Do not use chemicals that are incompatible with liquids sample O-rings. Sample and sealing capability damage can result in sample leakage and damage to the rotor housing and or the probe. Chemicals that are incompatible with liquids sample O-rings can compromise the integrity of the O-ring. Refer to the documentation supplied with the sampler kit or contact Varian Technical Assistance and request and request a list of sample O-ring chemical incompatibilities. CAUTION: Never use rotors that have been dropped onto a hard surface. Micro-cracks in the rotor material resulting from dropping can cause rotor explosions at low speeds. CAUTION: Spinning rotors heat up due to friction with air and can cause the sample to boil out of the rotor. Always purge the spinning system with VT flow to minimize the spin heating effect. 2 Sample Packing Procedure C 0907

4 Sizes and Sample Volumes Use the correct rotor and size rotor for the volume of sample. The correct rotor size and sample volume are listed in the following table: Size Sample Volume 4.0 mm 46 µl 4.0 mm 52 µl 5.0 mm 90 µl 5.0 mm 160 µl 6.0 mm 240 µl 7.5 mm 450 µl Sample Holder Parts and Tools Drive Tip and rotor wrenches press cap (white) Starter tool End cap Rubber disk Top sample Setting tool sleeve Flat bottom base (black) End cap press cap (brown) Push rod Bottom sample base (white) Sample cap (black) Extractor tool C 0907 Sample Packing Procedure 3

5 Packing the Sample CAUTION: Do not use chemicals that are incompatible with liquids sample O-rings. Refer to the documentation supplied with the sampler kit or contact Varian Technical Assistance and request a list of sample O-ring chemical incompatibilities. Inserting the Bottom Sample Spacer, page 4 Inserting the Drive Tip, page 5 Loading the Sample, page 5 Inserting the Top Sample Spacer, page 6 Inserting the End Cap, page 7 Inserting the Bottom Sample Spacer 1. Insert the tachometer end of an empty rotor sleeve into the black flat bottom base (B). sleeve Tachometer end (B) Sleeve 2. Place the black sample top cap on the rotor (D) and base. 3. Insert the bottom sample (solid) into the sample cap (E). 4. Use the short end of the setting tool (brown) to insert the sample into the rotor flush to the end of the rotor sleeve (F). 5. Remove the sample cap and check that the ends of the rotor and sample are flush (G). Sample cap (black) (E) (G) Cap Sample (black) Sleeve (D) (F) Cap Sample and sample must be flush Setting tool Sleeve Cap 4 Sample Packing Procedure C 0907

6 Inserting the Drive Tip 1. Insert the drive tip into the large end of the white starter tool. 2. Push (B) the drive tip into the rotor sleeve and push the bottom sample into the rotor sleeve. 3. Remove the starter tool. 4. Insert the rotor into the rotor sleeve base (black). Press tip into the rotor sleeve using the white drive tip press cap. Starter tool partially inserted into the rotor (B) Starter tool and sample press cap (white) CAUTION: s will be damaged if the wrong drive tip press cap is used to insert the drive tip. The angled surfaces of the drive tip press cap provided fit the corresponding drive tip. Other caps do not match and will damage the drive tip and compromise rotor spinning. 5. Remove the rotor and check that there are no gaps and (B) between the drive tip and rotor sleeve. The drive tip and rotor sleeve must be flush together. (B) Large gap sleeve Drive Tip Small gap sleeve Drive Tip No gap sleeve Drive Tip CAUTION: A gap between the rotor sleeve and drive tip may cause spinning failures and instabilities. Loading the Sample 1. Insert the rotor sleeve into the white drive tip base. 2. Use syringe or pipette to load the sample into the rotor. Pipette sleeve base (white) C 0907 Sample Packing Procedure 5

7 Inserting the Top Sample Spacer The top sample has an internal thread in one end that must face outward toward the end of the rotor sleeve during insertion. The extractor tool attaches to the thread to pull out the sample. 1. Place the black sample cap onto the white drive tip base and rotor sleeve. 2. Insert the top sample (B) into the black top cap with the threaded end facing outward. 3. Insert the sample into the rotor using the longer nose of the brown setting tool (B). A hole through the center of the sample allows removal of air and excess sample from the rotor. 4. Remove any sample that has extruded through the rear sample. 5. Check that the rear sample is approximately 4 mm inside the rotor before proceeding with the next step. Small hole Threaded end (B) Setting tool Top threaded end sleeve Cap Remove excess liquid Spacer set approximately 4 mm below the rotor top 6. Use the push rod (D) to push the top disk into the rotor sleeve until it is flat against the top sample. Do not push the top further into the rotor sleeve. (D) Push rod Top disk 6 Sample Packing Procedure C 0907

8 Inserting the End Cap 1. Place the threaded end of the end cap into the small end of the starter tool (B). (B) Starter tool 2. Insert the end cap into the rotor sleeve cone end first. 3. Remove the starter tool. sleeve End cap cone 4. Press the end cap into the rotor sleeve using the brown end cap press cap (D). (D) (E) End cap and sleeve are flush 5. Verify that the end cap and sleeve are flush (E). End cap press cap (brown) 6. Mark over the tachometer mark with a black permanent marker for the tachometer spin speed measurement (F). The tachometer system will not measure the rotor spin speed without a tachometer mark on the end of the rotor sleeve. (F) Tachometer marking C 0907 Sample Packing Procedure 7

9 Removing the Liquid Sample 1. Hold the extractor tool head. 2. Thread the end cap-rotor onto the extractor tool. 3. Rotate the extractor tool body to pull out the end cap from the rotor assembly (B). 4. Remove the end cap from the extractor tool. 5. Thread the top sample onto the extractor tool (D). 6. Rotate the extractor tool body to pull out the sample from the rotor assembly (B). 7. Remove the sample from the extractor tool. 8. Remove the sample using pipette or absorbent towel. Extractor tool head Extractor tool body End cap (E) Sample assembly assembly assembly (B) Extractor tool body (D) Extractor tool head (F) sleeve assembly assembly Pipette 9. Clamp the wrenches onto the drive tip and rotor (G). 10. Twist and pull the drive tip to remove it from the rotor sleeve. 11. Push the bottom sample out of the rotor sleeve using the push rod (H). (G) Drive tip wrenches (H) Bottom sample Push rod sleeve 8 Sample Packing Procedure C 0907

10 Packing Procedure for 4 to 7.5 mm Liquid Samples Sample Volumes of 46 to 450 µl Pub. No , Rev. C 0907 Technical contributor: Chuck Mullen Technical writer and editor: Everett Schreiber Revision History: A 0906 Initial release B0307 Updated to include 4 mm samples, ECO 07P0015 C0907 Updated to include 7.5 mm samples, ECO 07T0601 Copyright 2007, Varian, Inc Hansen Way, Palo Alto, California All rights reserved. Printed in the United States The information in this document has been carefully checked and is believed to be entirely reliable. However, no responsibility is assumed for inaccuracies. Statements in this document are not intended to create any warranty, expressed or implied. Specifications and performance characteristics of the software described in this manual may be changed at any time without notice. Varian reserves the right to make changes in any products herein to improve reliability, function, or design. Varian does not assume any liability arising out of the application or use of any product or circuit described herein; neither does it convey any license under its patent rights nor the rights of others. Inclusion in this document does not imply that any particular feature is standard on the instrument. MERCURYplus and MERCURY-VX are registered trademarks or trademarks of Varian, Inc. Other product names in this document are registered trademarks or trademarks of their respective holders C 0907 Sample Packing Procedure 9

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