Hach Micro Dist Operation And Application Manual
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Hach Micro Dist Operation And Application Manual

Hach Micro Dist Operation And Application Manual

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Catalog Number 01304
Micro Dist™ Operation and Applications
USER MANUAL
February 2009 Edition 5
© Hach Company, 2004–2009. All rights reserved. Printed in the U.S.A.

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  • Page 1 Catalog Number 01304 Micro Dist™ Operation and Applications USER MANUAL February 2009 Edition 5 © Hach Company, 2004–2009. All rights reserved. Printed in the U.S.A.
  • Page 2 Visit us at www.LachatInstruments.com...

  • Page 3: Table Of Contents

    2.1.1 Use of Hazard Information ....................7 2.1.2 Precautionary Labels ......................7 2.2 Principle of Operation ......................... 8 2.3 Distilling Calibration Standards with the Micro Dist System ............9 Section 3 Installation ......................11 3.1 Unpacking the Instrument ......................11 3.1.1 Micro Dist Setup .......................
  • Page 4 Section 18 Replacement Parts and Accessories ...............63 Section 19 Contact Information ...................65 Section 20 Limited Warranty ....................66 Appendix A Micro Dist Methods ..................67 A.1 Methods List ..........................67 Appendix B Troubleshooting ....................69 B.1 Common Problems, Likely Causes, and Possible Solutions ............69...

  • Page 5: Section 1 Specifications

    Relative Humidity Up to 92.5%, non-condensing Shelf Weight 20 kg (45 lb) Ordinary air-conditioned lab. Provide at least 6 inches distance between the Micro Dist Ventilation Needed block and all other vertical surfaces. Safety Laboratory 61010-1, 61010-2-010 (UL, CSA, EN Safety Standards)
  • Page 6 Visit us at www.LachatInstruments.com...

  • Page 7: Section 2 General Information

    Section 2 General Information 2.1 Safety Information Please read this entire manual before unpacking, setting up, or operating this equipment. Pay attention to all danger and caution statements. Failure to do so could result in serious injury to the operator or damage to the equipment. To ensure that the protection provided by this equipment is not impaired, do not use or install this equipment in any manner other than that specified in this manual.

  • Page 8: Precautionary Labels

    Cyanide–1, a digestion may take place as well. The Micro Dist™ system was developed for the analytical distillation of samples which are largely aqueous. In such samples an in situ steam distillation can be done simply by boiling the...

  • Page 9: Distilling Calibration Standards With The Micro Dist System

    The Micro Dist system strips analytical distillation down to its bare essentials. The sample is pipetted into a sample tube and sealed to a collector tube. This assembly is placed into a special heating block which fits it very closely, allowing the poor-conducting polypropylene to be heated rapidly yet locally.
  • Page 10 Micro Dist Method. Some tubes such as the phenolics method tube do not contain trapping solution. Be sure to use the Micro Dist tubes which match the Micro Dist Method. The Micro Dist Method will define the trapping solution;...

  • Page 11: Section 3 Installation

    • To move the Micro Dist, position a person on each side of the instrument. With both hands under the side, lift the analyzer simultaneously.
  • Page 12 Installation...

  • Page 13: Section 4 Operation

    4.1 Setting the Temperature 4.1.1 Heater Block CAUTION Burn hazard. The Micro Dist heater block top surface is a burn hazard at operating temperature. Wear heat-resistant gloves when putting tubes in or taking them out of the heating block. If a burn occurs, immediately put the burned area under cold running water for five minutes.

  • Page 14: Using Micro Dist™ Tubes

    Note: The maximum temperature set point of this equipment is 135 °C. 4.2 Using Micro Dist™ Tubes DANGER Fire hazard. Do not use the Micro Dist with flammable substances. DANGER Risque d'incendie. Ne pas utiliser le Micro Dist avec des substances inflammables.

  • Page 15: Filling And Assembling The User-Fill Collector Tubes

    Note: Do not refrigerate Micro Dist tubes. This will cause the membrane ring to shrink and the trapping solution to leak out. 4.2.1 Filling and Assembling the User-Fill Collector Tubes The User-Fill collector tube option is designed for the user who: •...
  • Page 16 6, discarding the old membrane. There is one extra membrane supplied for every 10 tubes in case this happens. 9. The collector tube is now ready to use with Micro Dist methods.
  • Page 17 Operation Figure 2 Collector Tube...
  • Page 18 Visit us at www.lachatinstruments.com...

  • Page 19: Section 5 Startup

    Risque de blessure personnelle. L'instrument doit toujours être soulevé ou déplacé par deux personnes. 1. Place the Micro Dist on a level surface, preferably under a fume hood. Leave at least six inches of clearance on all sides of the instrument to allow for ventilation and heat dissipation.
  • Page 20 Visit us at www.lachatinstruments.com...

  • Page 21: Section 6 Maintenance

    (122 °F) pour les parties métalliques est généralement considérée comme sans danger de brûlure au toucher. Clean the Micro Dist exterior by wiping down with water. Note: Before using any cleaning or decontamination method except those recommended by the manufacturer, contact the manufacturer to confirm that the proposed method will not damage the equipment.

  • Page 22: Calibrating The Automatic Re-Pipettor

    Important Note: 100–115 V models: Although there are positions for 2 fuses in the 100–115 V Micro Dist model, only the upper fuse in the fuse drawer is connected in the circuit. A spare fuse may be present in the lower slot, but it is not required.

  • Page 23: Section 7 General Procedure

    Table 2 describes the occupational threshold limits for gases that may potentially be released from the Micro Dist in a fault condition. Table 2 Hazardous gas information for specific methods Occupational...
  • Page 24 General Procedure In the following procedure, refer to the marks on the ends of the collector tube. means 'distillation’ or 'discarded' end and means 'measuring' end. See Figure 2 on page 1. Set the controller to temperature specified in method. Allow the heater block to warm up.
  • Page 25 General Procedure Figure 4 Adding the Releasing Solution 5. Immediately push the end of a collector tube over the open end of each sample tube to start the seal (Figure 6. Place the assembly in the press (Figure 5), putting the sample tube through the hole in the white base.
  • Page 26 General Procedure 7. The pressing motion should be a smooth constant pressure which is just enough to slide the sample tube inside the collector tube. A jerky, forced motion may cause added strain to the tube and could potentially crack it. Press down on the handle until the stop ring on the sample tube hits the end of the collector tube.
  • Page 27 General Procedure Figure 7 Placing the Collector Tube in the Rack 12. For each collector tube, hold the tube horizontally and rinse its walls with the distillate in order to homogenize it. Slowly roll the distillate around in the tube to gather all droplets clinging to the tube walls into the bulk of the distillate.
  • Page 28 General Procedure Figure 9 Breaking the ‘D’ End of the Collector Tube Figure 10 Discarding the ‘D' End 14. In the remaining end of the collector tube, dilute to the 6.0 mL mark with deionized water, or dilute to 10 mL. This results in the original sample volume.

  • Page 29: Micro Dist™ Method (Method Number 10-204-00-1-X)

    Micro Dist under a fume hood. DANGER Risque d'inhalation de produits chimiques. Pour éviter le contact potentiel avec du gaz de Cyanure d'hydrogène (HCN), le fabricant recommande d'utiliser le Micro Dist sous une hotte aspirante. CAUTION Chemical hazard.

  • Page 30: Releasing Agent

    Cyanide–1 10. Put on the heat-resistant gloves. Push the sample tube and end of each tube all the way into the preheated block so that the collector tube stop ring touches the block. Placing 21 tubes should take less than one minute. 11.

  • Page 31: Sources

    Cyanide–1 200 mL of 7.11 M sulfuric acid / 0.79 M magnesium chloride recipe: 1. In the hood, place a 500 mL beaker on a top-loading balance with a 400 g capacity or greater. It is best to do this in the hood as HCl fumes will be released.

  • Page 32: Calculations Showing Equivalency Of Concentrations Of Releasing Solutions

    Note: More than 0.060 mL of chloramine T will prevent the color from developing with pyridine-pyrazolone. 8.5 Calculations Showing Equivalency of Concentrations of Releasing Solutions Equivalency of releasing solutions in Micro Dist Method Cyanide–1 and in USEPA Method 335.2 (see section 8.3 on page 33).

  • Page 33: Calculations Showing Equivalency Of Concentrations Of Trapping Solution

    Method 335.2. 8.6.1 Micro Dist Method Cyanide–1 In the Micro Dist Method, 1.5 mL of 1.0 M NaOH becomes 6.0 mL solution after distillation and dilution to the mark: 1.0 M NaOH x (1.5 mL / 6.0 mL) = 0.25 M NaOH 8.6.2 USEPA Method 335.2...
  • Page 34 Visit us at www.lachatinstruments.com...

  • Page 35: Micro Dist™ Method

    Micro Dist under a fume hood. DANGER Risque d'inhalation de produit chimique. Pour éviter le contact potentiel avec du gaz de Cyanure d'hydrogène (HCN), le fabricant recommande d'utiliser le Micro Dist sous une hotte aspirante. CAUTION Chemical hazard. Always follow appropriate laboratory safety procedures when handling chemicals.
  • Page 36 Cyanide–2 8. Immediately push the end of a Cyanide–1 collector tube over the open end of each sample tube to start the seal. 9. Place the assembly in the press, putting the sample tube through the hole in the white base. Before pressing the user should grip the collector tube firmly at the breakaway point to keep the tube from shifting during the pressing procedure.

  • Page 37: Section 10 Cyanide-3 (Wad)

    Micro Dist under a fume hood. DANGER Risque d'inhalation de produit chimique. Pour éviter le contact potentiel avec du gaz de Cyanure d'hydrogène (HCN), le fabricant recommande d'utiliser le Micro Dist sous une hotte aspirante. CAUTION Chemical hazard. Always follow appropriate laboratory safety procedures when handling chemicals.
  • Page 38 Cyanide–3 (WAD) 7. Immediately push the end of a Cyanide–3 collector tube over the open end of each sample tube to start the seal. 8. Place the assembly in the press, putting the sample tube through the hole in the white base. Before pressing the user should grip the collector tube firmly at the breakaway point to keep the tube from shifting during the pressing procedure.

  • Page 39: Releasing Agent

    Cyanide–3 (WAD) 10.2 Releasing Agent 1 L of 0.87 M acetic acid / 0.50 M zinc acetate / 0.52 M sodium acetate Make this releasing solution in a 1 L container and then place it directly in the automatic re-pipettor supplied with the starter kit. This is enough to treat 1300 samples.
  • Page 40 Visit us at www.lachatinstruments.com...

  • Page 41: Micro Dist™ Method

    Micro Dist under a fume hood. DANGER Risque d'inhalation de produit chimique. Pour éviter le contact potentiel avec du gaz de Cyanure d'hydrogène (HCN), le fabricant recommande d'utiliser le Micro Dist sous une hotte aspirante. CAUTION Chemical hazard. Always follow appropriate laboratory safety procedures when handling chemicals.
  • Page 42 Cyanide–5 to the sample tube using the supplied automatic pipet. See section 8.2 on page 32 for this recipe. 7. Immediately push the end of a Cyanide–5 collector tube over the open end of each sample tube to start the seal.

  • Page 43: Section 12 Phenolics-1

    This is a method for distilling samples containing 0.002 to 50.0 mg phenolics/L with the Micro Dist distillation apparatus. In the following procedure, refer to the marks on the ends of the collector tube.

  • Page 44: Sources

    Phenolics–1 sample tube using a downward, twisting motion as opposed to a sideways motion. Remove the sample tube within 4 seconds of removing it from the block or suck-back of the sample will occur. Dispose of the sample tube and the hot solution left in it by dropping it into the sink or waste bucket.

  • Page 45: Section 13 Sulfide-1

    Micro Dist under a fume hood. ATTENTION Risque d'inhalation de produit chimique. Pour éviter le contact potentiel avec du gaz de sulfure d'hydrogène (H2S), le fabricant recommande d'utiliser le Micro Dist sous une hotte aspirante. CAUTION Chemical hazard. Always follow appropriate laboratory safety procedures when handling chemicals.
  • Page 46 Sulfide–1 required may be more than 0.45 mL. See section 13.3 on page 49 further details. 6. Immediately push the end of a Sulfide–1 collector tube over the open end of each sample tube to start the seal. 7. Place the assembly in the press, putting the sample tube through the hole in the white base.

  • Page 47: Releasing Agent

    Sulfide–1 13.2 Releasing Agent 300 mL of 9.0 M sulfuric acid releasing agent for the Sulfide–1 Method: Make this releasing solution up in a beaker under the hood and transfer to the automatic re-pipettor supplied with the starter kit after cooling.

  • Page 48: Comparison Of This Method And Sw-846 Method 9030B, Revision 2

    Sulfide–1 13.4 Comparison of this method and SW–846 Method 9030B, Revision 2 Both methods use a trapping solution which is 0.043 M in zinc acetate and which contains 1.60% formaldehyde. The stock 37% formaldehyde solution contains 10–15% methanol. 2.0 mL of this solution is in each Sulfide–1 collector tube.

  • Page 49: Section 14 Sulfide-2

    This is a method for distilling samples containing 0.01-10.0 mg acid soluble S/L with the Micro Dist distillation apparatus, for colorimetric determination. In the following procedure, refer to the marks on the ends of the collector tube.
  • Page 50 Sulfide–2 required may be more than 0.45 mL. See section 14.2 on page 53 further details. 6. Immediately push the end of a Sulfide–2 collector tube over the open end of each sample tube to start the seal. 7. Place the assembly in the press, putting the sample tube through the hole in the white base.

  • Page 51: Sources

    14.3 Releasing Agent 300 mL of 9.0 M sulfuric acid releasing agent for the Sulfide–2 Micro Dist Method: Make this releasing solution up in a beaker under the hood and transfer to the automatic re-pipettor supplied with the starter kit after cooling.
  • Page 52 Visit us at www.lachatinstruments.com...

  • Page 53: Section 15 Ammonia-1: Phenate Method/Ise

    This is a method for distilling samples containing 0.010 to 2.0 mg N/L with the Micro Dist distillation apparatus. In the following procedure, refer to the marks on the ends of the collector tube.
  • Page 54 Ammonia–1: Phenate Method/ISE the collector tube stop ring touches the block. Placing 21 tubes should take less than one minute. 10. Set the timer for 30 minutes. 11. When 30 minutes is up, put on the heat-resistant gloves. Remove the first tube from the block and immediately pull off its sample tube using a downward, twisting motion as opposed to a sideways motion.

  • Page 55: Borate Buffer

    Ammonia–1: Phenate Method/ISE 15.2 Borate Buffer Make this buffer solution up in a 1 L container and then place directly in the automatic re-pipettor supplied with the starter kit. This will make 1 L of 0.011 M Na . This is enough to treat 1300 samples.
  • Page 56 Visit us at www.lachatinstruments.com...

  • Page 57: Section 16 Ammonia-2: Nesslerization Method

    This is a method for distilling samples containing 0.010 to 2.0 mg N/L with the Micro Dist distillation apparatus. In the following procedure, refer to the marks on the ends of the collector tube.

  • Page 58: Borate Buffer

    Ammonia–2: Nesslerization Method 11. When 30 minutes is up, put on the heat-resistant gloves. Remove the first tube from the block and immediately pull off its sample tube using a downward, twisting motion as opposed to a sideways motion. Remove the sample tube within 4 seconds of removing it from the block or suck-back of the sample will occur.

  • Page 59: Section 17 Tritium-1

    Section 17 Tritium–1 17.1 Micro Dist™ Method CAUTION Chemical hazard. Always follow appropriate laboratory safety procedures when handling chemicals. Always wear personal protective equipment appropriate for the chemicals you are handling. ATTENTION Danger chimique. Suivez toujours les procédures de laboratoire de sécurité lors de l'utilisation de produits chimiques.

  • Page 60: Sources

    Tritium–1 10. When 90 minutes is up, put on the heat-resistant gloves. Remove the first tube from the block and immediately pull off its sample tube using a downward, twisting motion as opposed to a sideways motion. Remove the sample tube within 4 seconds of removing it from the block or suck-back of the sample will occur.

  • Page 61: Section 18 Replacement Parts And Accessories

    Sample Tube Rack, 60 tube capacity 17011 Step-Up Transformer (110 V to 220 V), non-CE models only 17020 Timer 17021 Tube Press Assembly 17023 The starter kit includes one set of 21 Micro Dist tubes with the purchase of the Micro Dist block.
  • Page 62 Visit us at www.lachatinstruments.com...

  • Page 63: Section 19 Contact Information

    Brief description or model number • Quantity International Customers Hach maintains a worldwide network of dealers and distributors. To locate the representative nearest you, send an e-mail to: intl@hach.com or contact: Hach Company World Headquarters; Loveland, Colorado, U.S.A. Telephone: (970) 669-3050; Fax: (970) 461-3915 Technical and Customer Service (U.S.A.

  • Page 64: Section 20 Limited Warranty

    Section 20 Limited Warranty Lachat Instruments, a Hach Company Brand, warrants its products to the original purchaser against any defects that are due to faulty material or workmanship for a period of *one year* from date of shipment unless otherwise noted in the product manual.

  • Page 65: Appendix A Micro Dist Methods

    Appendix A Micro Dist Methods A.1 Methods List Table 3 for descriptions of the Micro Dist methods. See Table 4 for a list of related QuikChem methods. Table 3 Micro Dist Methods Summary Micro Dist Matrix and Collector Tube Trapping Solution...
  • Page 66 Micro Dist Methods Table 3 Micro Dist Methods Summary Micro Dist Matrix and Collector Tube Trapping Solution Assembled User-Fill User-Fill User-Fill Method No. Chemistry Recipe Pkg/21 Pkg/10 Pkg/50 Pkg/100 contaminated A17014 Tritium–1 No trapping solution. waters, solids (pkg of 10)

  • Page 67: Appendix B Troubleshooting

    Appendix B Troubleshooting B.1 Common Problems, Likely Causes, and Possible Solutions Very low or erratic recoveries The most common cause of very low or erratic recoveries is that the tubes are not being pushed all the way into the block. It is not enough to simply let them drop into the holes.
  • Page 68 Experiment with samples to determine the best weight of sample to add for each matrix type. The sample will be diluted with DI water (5 to 6 mL) per the Micro Dist manual. Calculating the amount of sample in mg/kg after analysis: Multiply the determined concentration in mg/L by (1 L / l000 mL) * dilution vol.
  • Page 69 Troubleshooting If foaming or caking of the membrane continues to be a problem even with reduced sample weights of 0.5 g, try the following: • Add activated charcoal so it covers the surface of the solid and then fill the remaining void space with glass wool.
  • Page 70 Visit us at www.lachatinstruments.com...

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