Environmental Express CURRENT User Manual

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HotBlock™ Digestion System

Operation & Instruction Manual

Call 800.343.5319 or 843.881.6560 • www.environmentalexpress.com

HotBlock™: Operation and Instruction Manual Contents

Dear Valued Customer,

Thank you for purchasing a

HotBlock™ Digestion System from

Environmental Express.

We pride ourselves on

providing innovative

products designed

to improve accuracy,

efciency, and safety

in your laboratory. Please take some

time to read your product manual

before using your HotBlock™.

As always, our Technical Sales

and Technical Support Teams are

available to assist with any questions

you have regarding our products.

Best Regards,

Al Jurgela

Chief Executive Ofcer

Environmental Express, Inc.

Contents

General Information

Warranty and Repair Policy 1 Declaration of Conformity 2

About Your HotBlock™

50mL HotBlock™ Specications 3 15mL HotBlock™ Specications 4 100mL HotBlock™ Specications 4

Getting Started

HotBlock™ Information and Markings 5 Unpacking and Installation 6 HotBlock™ Temperature Information 7 Potential Hazards and Maintenence 8

Care and Maintenance of Your HotBlock™

Circuitry Diagram 9 HotBlock™ Replacement Parts 10 Troubleshooting Your Block 11-13

Adaptation of EPA Methods for Use with Your HotBlock™

EPA Approval Letter 14 Method 200.2, Revision 2.8 15-16 Method 200.7 17-18 Method 200.8 19-20 Methods 245.1, 7470, and 7471 for Mercury Digestions 21-22 Method 365.2 for Phosphorus 23-24 Method 3050B 25-26 NIOSH Method 7303 27 Sample Preparation for Lead Analysis Using the GhostWipe 28-29 Method 3060 for use with the HotBlock™ and StirBase Systems 30-31

HotBlock™ Parts and Supplies

50mL HotBlock™ Accessories and Consumables 32-33 100mL HotBlock™ Accessories and Consumables 34 15mL HotBlock™ Accessories and Consumables 35 AirLite HEPA-Filtered Enclosure 36 Sample Filtration Supplies 36-37 GhostWipes for Surface Sampling 38

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HotBlock™: Operation and Instruction Manual Warranty and Repair Policy

Limited Warranty

The Environmental Express HotBlockTM is warranted against defects in materials and workmanship when used in accordance with applicable instructions, for a period of one year from the date of shipment. This warranty extends to parts, labor, and any approved transportation charges. This warranty applies only to damage or failure caused by normal laboratory use. The warranty is limited to product repair. If Environmental Express is unable to repair the HotBlock, the customer may, at his or her option, receive a replacement unit or a full refund. Operating the HotBlockTM at temperatures higher than 150°C will void the warranty.

Environmental Express makes no other warranty, expressed or implied for this product with respect to merchantability, tness for a particular use or any other matter. Environmental Express is not liable for any consequential or compensatory damages arising from use of, or in conjunction with this product. The maximum liability shall be the invoice price of this product.

Repair Policies

Under Warranty Repair:

If the HotBlock™ should fail to operate within the warranty period (one year from date of shipment) Environmental Express will repair it and ship it back to the customer at our expense. The remainder of the warranty period will be honored from the original ship date. Environmental Express will bear the cost of ground transportation both to and from the customer’s location, and bear the cost of any parts, labor and cleanup required. However, if it is determined that the damage to the HotBlock™ was caused by negligence or improper use, this warranty will not apply. The warranty is also void if the system is used beyond its intended purpose or in the event of any unauthorized repair. In such cases, reasonable and customary repair charges will apply. Repair charges will be quoted prior to work being done.

Loaner HotBlocks™ MAY be available during the repair period. There are only a limited number of these units. A reasonable charge for “cleanup” will be charged if a loaner is issued. The customer will be responsible for all shipping charges associated with a loaner unit.

Out of Warranty Repair:

If the HotBlock™ fails after the warranty period has lapsed, the repair procedure is as follows:

First, notify an Environmental Express Technical Service Representative of product’s failure and place an order for repair. Whenever possible, our customer service technician will walk you through possible troubleshooting scenarios which may enable you to repair your block on site. (See the troubleshooting section of this manual, pages 11-13).

If on site repair is not possible, the customer may return the non-working unit to Environmental Express using appropriate shipping containers and insurance. Repair charges will be assessed and estimated prior to work being done. Repair charges will include all freight costs as well as reasonable and customary charges for parts and labor.

Call 800.343.5319 or 843.881.6560 • www.environmentalexpress.com

2345 A Charleston Regional Pkwy • Charleston, SC 29492

Product Information:

Item # Date of Purchase

HotBlock™ Serial #

Please record the serial # of your HotBlock™ here for easy reference. Your serial # is located on the back of your HotBlock™.

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HotBlock™: Operation and Instruction Manual Declaration of Conformity

The manufacturer, Environmental Express, 2345A Charleston Regional Parkway, Charleston, SC 29492 declares that the following products, HotBlock™ Catalog Numbers, SC196, SC154, SC150, SC151, SC100, and C6002, are in conformity with:

Standard for Safety Electrical Equipment for Measurement, Control, and Laboratory Use; Part 1 General Requirements, UL 61010-1, CAN/CSA-C22.2 No. 61010-1, 2nd Edition, Issued 12 July, 2004 with revisions through and including 28 October, 2008; Equipment for Measurement, Control, and Laboratory Use Part 2-010: Particular Requirements for Laboratory Equipment for the Heating of Materials, IEY 61010-2-010, 2nd Edition, Issued 1 June, 2003, Safety Requirements for Electrical Equipment for

4000040

Environmental Express, Inc. declares that all HotBlocks conform with the essential requirements of the applicable EC directives.

Measurement, Control, and Laboratory Use - Part 2-010:Particular Requirements for Laboratory Equipment for the Heating of Materials, CSA C22.2.61010.2.01

Signed: ________________________________________

Al Jurgela, Chief Executive Ofcer

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HotBlock™: Operation and Instruction Manual 50mL HotBlock™ Specications

HotBlocks™ for 50mL Samples

36-Well 50mL HotBlock™

SC100:

Nominal Sample Size: 50mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 15" x 15"

Crated Size: 23" x 23" x 17"

Weight: 43 lb.

Shipping Weight: 58 lb.

Electrical: 120VAC*, 9A

Sample Capacity: 36

Racks Included: SC200 (2)

54-Well 50mL HotBlock™

12-Well 50mL HotBlock™

* All HotBlocks™ are also available in 240V.

SC154:

Nominal Sample Size: 50mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 15" x 21.5"

Crated Size: 26" x 23" x 17"

Weight: 59 lb.

Shipping Weight: 78 lb.

Electrical: 120VAC*, 14A

Sample Capacity: 54

Racks Included: SC200 (3)

C6002:

Nominal Sample Size: 50mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 8.55" x 18.5"

Crated Size: 22" x 19" x 13"

Weight: 30 lb.

Shipping Weight: 35 lb.

Electrical: 120VAC, 13A

Sample Capacity: 12

Racks Included: C6050 (1)

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HotBlock™: Operation and Instruction Manual 15mL and 100mL HotBlock™ Specications

HotBlocks™ for 15mL Samples

96-Well 15mL HotBlock™

SC196:

Nominal Sample Size: 15mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 15" x 21.5"

Crated Size: 26" x 23" x 17"

Weight: 59 lb.

Shipping Weight: 80 lb.

Electrical: 120VAC*, 13A

Sample Capacity: 96

Rack Set Included: SC296

HotBlocks™ for 100mL Samples

25-Well 100mL HotBlock™

35-Well 100mL HotBlock™

* All HotBlocks™ are also available in 240V.

SC150:

Nominal Sample Size: 100mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 15" x 15"

Crated Size: 23" x 23" x 17"

Weight: 42 lb.

Shipping Weight: 54 lb.

Electrical: 120VAC*, 9A

Sample Capacity: 25

Rack Set Included: SC225

SC151:

Nominal Sample Size: 100mL

Temperature Range: to 150ºC

Thermocouple: Type K

Footprint: 15" x 21.5"

Crated Size: 26" x 23" x 17"

Weight: 59 lb.

Shipping Weight: 65 lb.

Electrical: 120VAC*, 13A

Sample Capacity: 35

Rack Set Included: SC235

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HotBlock™: Operation and Instruction Manual HotBlock™ Information and Markings

Environmental Express HotBlock™

Environmental Express HotBlocks™ provide an efcient method of digesting and storing water, wastewater, soil and sludge samples for metals analysis. These innovative digestion systems allow samples to be digested in a corrosion-free environment. In addition, samples are handled in a small area with minimal radiant heat loss. Users should be aware of potential dangers from heating certain types of compounds. Such hazards may include explosion or the release of toxic or ammable gases.

Denitions/Markings

Each HotBlock™ displays certain markings and symbols. All personnel working with the HotBlocks™ should have an understanding of the following symbols and denitions:

• V = voltage

• ~ = alternating current

• Hz = frequency

• A = amperes

This symbol means Caution Hot Surface. The surface of the HotBlock™ may be too hot to safely touch with bare hands.

This symbol means Read

and become familiar with instructions before operation of instrument.

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HotBlock™: Operation and Instruction Manual Unpacking and Installation

Unpacking Your HotBlock™:

1. Remove the HotBlock™ from the shipping container by lifting from the bottom of the block. The lid should not be used for lifting.

2. Your HotBlock™ is shipped with metal screws securing the bottom panel. The metal screws must be removed before operating your HotBlock™. Remove the metal screws and replace them with the PVC screws and rubber feet included with your shipment. The corrosion-resistant PVC screws and rubber feet are designed to secure the bottom plate.

Important: Do not over tighten the PVC screws!

Installation Requirements

Locate the HotBlock™ under a fume hood with a minimum face velocity of 100fpm, and allow a minimum of 2" of space on all sides. The following environmental conditions should be observed:

• Ambient temperature range: 5-30°C

• Ambient relative humidity: 0-90%RH

• Altitude: sea level to 2500 meters

HotBlocks™ are rated as Pollution Degree 2 and Installation Category 2.

Electrical Requirements

Required Voltage: 120 volts, ~60Hz, 15A (all HotBlocks™ are also available in 240V with CE mark)

Power should not vary greater than±10%. Use the supplied heat-resistant power cord or equivalent to connect to the power supply.

For safety reasons, a separate power receptacle should be provided for each unit in the system. Do not use extension cords or outlet adaptors. Make certain that power outlets are earth-grounded at the grounding pin.

See individual specications for each HotBlock™ model, pages 3-4.

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HotBlock™: Operation and Instruction Manual HotBlock™ Temperature Information

HotBlock™ Temperature Settings:

The pre-set factory “set point” temperature of your HotBlock™ is 106°C. Factory tests have shown that this temperature is “sea level safe.” Liquids in uncovered polypropylene tubes should not boil at this setting. Please note that the set point of the block is not the same as the temperature of the liquids being digested. The block temperature should be optimized for the specic digestion. The temperature of liquid contents of the digestion cup will vary according to:

• The material being digested

• The number of samples being digested

• The air movement of the digestion area

• The addition of a watch glass or reux cap

If watch glasses are being used, the control point temperature should be lowered approximately 10°C to avoid boiling.

Note: The maximum sample temperature tolerance for our polypropylene digestion vessels (SC475) is 130°C.

Remember that the temperature display (current block temperature) is not the temperature of the sample. Sample temperature will usually be 5-15° less than the display temperature.

Adjusting the Temperature of Your HotBlock™:

1. Plug the HotBlock™ into an approved receptacle. Turn the HotBlock™ on by pressing the button on the back of the unit. Wait until the display shows the current block temperature (in red) and the set point temperature (in green).

2. Press and hold or tap the  or  key. The display will show the set point temperature on the right in blue. The adjustment is from ambient to 150°C in increments of 0.1°C. There is no need to press the green (advance) or ∞ button.

Safe-Sample™ Temperature Protection:

Your HotBlock™ is protected from runaway temperatures by a fail-safe alarm system. In the unlikely event that the heating system fails to respond to the controller, the Safe-Sample™ system will automatically shut the system off and sound an audible alarm.

This alarm sequence occurs if the actual temperature of the block reaches a temperature that is fteen degrees higher than the set point temperature. If this should occur, the HotBlock™ will stop heating, preventing the loss of samples. The HotBlock™ must be turned off, then turned back on to reset the alarm.

If the alarm sounds, see the troubleshooting section of this manual, page 11-13.

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HotBlock™: Operation and Instruction Manual Potential Hazards and Maintenance

Potential Hazards:

The HotBlock™ should only be operated by properly trained personnel using standard laboratory safety practices.

Use extreme caution when operating the HotBlock™. Plastic and graphite surfaces of the HotBlock™ may be too hot to safely touch with bare hands.

The HotBlock™ contains electrical circuits and devices and compounds operating at dangerous voltages. Contact with these circuits, devices and components can cause serious injury or painful electric shock.

Proper grounding is essential to avoid a potentially serious electric shock hazard. Ensure that there is an internal ground connection between the metal base of the system and the 3-pin, earth-grounded receptacle.

For safety reasons a separate power outlet receptacle should be provided for each unit in the system. Do not use extension cords or outlet adaptors. Make certain each power outlet is earth-grounded at the grounding pin.

See individual block specications for power requirements, pages 3-4.

Application of the wrong supply voltage can create a re hazard and a potentially serious shock hazard, and could seriously damage the HotBlock™ system. See specications for individual HotBlocks™.

Users should be aware of potential dangers from heating certain types of compounds. Such dangers may include explosion or the release of toxic or ammable gases.

Always lift the HotBlock™ from the bottom of the unit.

Maintenance:

Any service inquiries should be directed to Environmental Express Technical Service Department.

After each use, clean exterior surfaces with a damp sponge to remove acid residue.

For acid spills, sponge with a diluted solution of sodium bicarbonate followed by distilled water. Acid that is spilled directly into the digestion wells should be neutralized and removed.

Before using any cleaning or decontamination methods except those recommended, check with Environmental Express to conrm the proposed method will not damage your HotBlock™.

Avoid excessive spills, as liquid allowed to overow into the HotBlock™ casing can severely damage electronic components.

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HotBlock™: Operation and Instruction Manual Circuitry Diagram

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HotBlock™: Operation and Instruction Manual HotBlock™ Replacement Parts

HotBlock™ Replacement Parts

Description Catalog #

Power module (plug receptacle) w/ push button switch SC941

Power Cord- heavy duty SC958

Environmental Express Controller SC945-W

12" X 12", 120V, silicone rubber, etched-foil heater mat for models SC100 & SC150 SC951

12" X 12", 240V, silicone rubber, etched-foil heater mat for models SC100-240 & SC150-240 SC951-240*

110/220V, 25A solid state relay SC952

Type K Thermocouple SC953

Terminal board SC955

Ceramic ber insulation for models SC100 & SC150 SC959

14" X 14" Powder-coated aluminum bottom for models SC100 & SC150 SC963

12" X 18", 120V, silicone rubber, heater mat for models SC154 and SC196 & SC151 SC966

12" X 18", 240V, silicone rubber, heater mat for models SC154-240 SC196-240 & SC151-240 SC966-240*

15" X 5" 120V silicone rubber heater mat for model C6002 (12-Place Block) C6300

15" X 5" 120V silicone rubber heater mat for model C6002-240 (12-Place Block) C6300-240*

Fail-Safe Relay SC968

Alarm Buzzer SC969

Ceramic ber insulation for models SC154, SC196 and SC151 SC970

14" X 19", powder-coated aluminum bottom for models SC154, SC196 and 151 SC971

PVC screw for rubber foot SC964

Rubber foot SC976

*for HotBlocks™ shipped outside the United States and Canada

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HotBlock™: Operation and Instruction Manual Troubleshooting Your Block

HotBlock™ Troubleshooting Guide:

Please consult the following troubleshooting guide if you experience problems with your HotBlock™. See wiring schematic (page 9) for component identication. If you are unable to resolve the problem or if replacement components are necessary, please contact technical service at 1-800-745-8218 as component replacement varies in degree of difculty. We recommend that only qualied personnel attempt troubleshooting electrical components.

When the HotBlock™ is initially powered on, the controller will cycle through a self-test sequence. It will then display the current temperature and begin heating until it reaches your set point temperature, where it will hold until the unit is powered off. The set point may be changed at any time. A change in the controller’s factory default settings or a failed component may cause the HotBlock™ to perform unsatisfactorily or render it inoperable.

The controller digital display will not illuminate.

There are two possible reasons that your controller will not illuminate.

1. The controller is not getting voltage or;

2. The controller itself has failed internally.

The problem can be effectively diagnosed by determining if the controller is or is not getting voltage using the following steps:

1. Conrm that the power cord is plugged securely into the HotBlock™ receptacle and a working outlet.

2. Conrm that the switch is in the “on” position. Press button on the back of HotBlock™.

3. Check the fuse located in the power module: a. Locate the fuse drawing indented into the power module next to the

socket.

b. Using a small screwdriver, pry open the fuse compartment cover.

c. Examine the exposed fuse for a break in the lament and if necessary,

check for continuity using a volt-meter.

d. If the fuse is determined to be blown, replace it with the spare fuse

located in the slide-out compartment beneath the operating fuse.

Caution: This procedure is a potential electrical hazard and should only be performed by qualied personnel.

4. Inside the HotBlock™, check voltage leading from the power module to the controller:

a. Remove the bottom panel of the HotBlock™ by unscrewing the rubber

feet.

b. On the back of the controller, locate the black wire at terminal 98 and

white wire at terminal 99. c. Set your volt-meter on AC voltage. d. Touch your red lead to the exposed white wire and black lead to the

exposed black wire. e. If your volt-meter reads 110-122V, the controller is receiving power but

has failed internally. It must be replaced (see parts list, page 10). f. If your volt-meter registers less than 110-122V, using step d above check

the black and white wires at the terminal board and then at the power

module to determine if there is a faulty connection.

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HotBlock™: Operation and Instruction Manual Troubleshooting Your Block

The audible alarm has sounded immediately after powering on and the HotBlock™ will not heat.

The temperature has overshot the set point and the audible alarm has sounded.

There are two possible causes for your HotBlock™ to sound the alarm immediately after the controller cycles through the self test. These are:

1. Your set point has been set to a value (≥) 15° less than ambient or current set point temperature. Turn the set point to within 15° of the actual temperature (blue numbers)

2. The controller is faulty. Call Environmental Express at 1-800-745-8218 for more information.

The function of the fail-safe system is to cease heating of the HotBlock™ in the event of a set point overshoot of 15°C and to alert the technician of the incident.

The HotBlock™ can be “fooled” into fail-safe mode if the set point is manually changed to a value ≥15° below your current temperature. However, the primary cause for the runaway temperature is a faulty relay that has exceeded its useful life.

You may troubleshoot the relay by following these steps:

Caution: This procedure is a potential electrical hazard and should only be performed by qualied personnel.

1. Power off your HotBlock™.

2. Remove the bottom panel of the HotBlock™ by unscrewing the rubber feet.

3. Power the HotBlock™ on and allow it to overshoot your set point temperature.

4. Locate the solid state relay mounted to the bottom panel.

5. Set your volt-meter to measure AC voltage.

6. Touch your red lead to terminal T1 (white wire) of the solid state relay and touch your black lead to a ground source (e.g., the green/yellow wire from the power module or an empty terminal on the terminal board).

7. If your volt-meter reads 110V-122V, then the relay is stuck in the “closed” position and it must be replaced (see parts list, page 10).

The temperature controller is performing erratically or displays an error message.

-OR-

The temperature controller is ashing Er.L Attn- Thermocouple

First reset default settings:

1. Hold the up and down arrow buttons for six seconds until Ai Set appears

2. Hold the down arrow until glbl set is in the window

3. Press the green advance key to enter

4. Continue pressing the green advance key until none user appears.

5. Press the down arrow key until Set1 user appears.

6. Pressing the advance key will restore default settings.

Fault

To troubleshoot the thermocouple, follow these steps:

1. Power off your HotBlock™.

2. Remove the bottom panel of your HotBlock™ by unscrewing the rubber feet.

3. Locate the thermocouple wires at terminals R1 (yellow) and S1 (red) of the controller and remove using a small screwdriver.

4. Cut the exposed ends of the two wires.

5. Strip 1/4" of insulation from each wire and reconnect them to the appropriate controller terminal and tighten.

6. Power on your HotBlock™.

7. If your display continues to ash Er.1 Attn- the thermocouple is faulty and must be replaced (see parts list, page 10).

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HotBlock™: Operation and Instruction Manual Troubleshooting Your Block

The HotBlock™ will not heat beyond ambient temperature.

A HotBlock™ that will not heat beyond ambient temperature typically has a failed relay, heater mat or controller.

Relay: To test the relay, the output voltage must be determined with a volt-meter.

Caution: This procedure is a potential electrical hazard and should only be performed by qualied personnel.

To measure the relay voltage, follow these steps:

1. Remove the bottom panel of your HotBlock™ by unscrewing the rubber feet.

2. Locate the solid state relay mounted to the bottom panel.

3. Set your volt-meter to measure AC voltage.

4. Touch your red lead to terminal T1(white wire) of the solid state relay and touch your black lead to a ground source (i.e., the green/yellow wire from the power module or an empty terminal on the terminal board).

5. If your volt-meter does not read 110V-122V, then the relay has stuck in the open position and it must be replaced (see parts list, page 10).

Heater Mat: To test the heater mat, the resistance in ohms (Ω) must be determined with a volt-meter. It is recommended that your heater mat be replaced if it measures 25 ohms (Ω) or greater. It is also recommended that the thermocouple and insulation be replaced as well, both are inexpensive parts that are not easily accessible otherwise.

To measure your heater mat resistance, follow these steps:

1. Power off your HotBlock™ and remove the bottom panel of your HotBlock™ by unscrewing the rubber feet.

2. Locate and disconnect the white wire connected to terminal T1 of the relay and an identical wire on terminal #2 of the terminal board (note: terminal #2 of the terminal board contains 3 white wires. To ensure you have the correct wire, trace it back and ensure it originates from the graphite portion of your HotBlock™.

3. Set your volt-meter to measure ohms (Ω)

4. Touch the red lead to one of these wires and touch the black lead to the remaining wire.

5. If your reading is “OL” (over limit) or a value greater than 25 ohms, then the heater mat has failed and it must be replaced (see parts list, page 10).

Controller: To test the controller, the output voltage must be determined with a volt-meter.

Caution: This procedure is a potential electrical hazard and should only be performed by qualied personnel.

To measure voltage from the controller, follow these steps:

1. Remove the bottom panel of your HotBlock™ by unscrewing the rubber feet.

2. Locate the solid state relay mounted to the bottom panel.

3. Set your volt-meter to measure DC voltage.

4. Touch the red lead to terminal A1 (red) and the black lead to terminal A2 (blue) of the solid state relay.

5. Your volt-meter should read 3V-16V.

6. If your volt-meter does not read 3V-16V, perform steps 3 and 4 on the red and blue (5 and 6) wires at the terminal board and controller to determine if there is a faulty or loose connection.

7. If you do not get a reading of 3V-16V at terminals Y2 (red) and W2 (blue) of the controller then the controller has failed internally and it must be replaced (see parts list, page 10).

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HotBlock™: Operation and Instruction Manual EPA Approval Letter

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HotBlock™: Operation and Instruction Manual EPA Method 200.2, Revision 2.8

Adaptation for EPA Method 200.2, Revision 2.8 for use with the Environmental Express HotBlock™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA digestion procedure 200.2 for use with the Environmental Express HotBlock™. EPA Method 200.2 is for the determination of total recoverable analytes in groundwater, surface water, drinking water, wastewater and (with the exception of silica) in solid samples such as sediment, sludge and soil. Use EPA Method 200.2 for reference while following the sample preparation steps outlined below. A complete list of elements appropriate for analysis is included in EPA Method 200.2. Analysis can be performed by ame atomic absorption, GF/AA, ICP and ICP-MS.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Number SC100, SC150* or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

2.4 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

*Note: For all procedures, when using the SC150 block with the SC490 digestion vials with

a 100mL sample, double the volume of all reagents and acids added.

3.0 Procedure, Aqueous Sample Preparation

3.1 Mix sample thoroughly to achieve homogeneity. For each digestion procedure, transfer a 50mL sample (or appropriate volume for your lab) into the SC475 polypropylene vessel. For best results, weigh the sample directly in the vessel on a tared balance.

3.2 Add 1mL (1:1) HNO3 and 0.5mL (1:1) HCl, then swirl. Heat the sample in the HotBlock™ at 95°C for 2.5 hours without boiling. Place a ribbed watch glass (SC505) on top of the digestion vessel.

Note: When using a watch glass, adjust the control point temperature of the HotBlock™

so that a 50mL, 5% acid solution is heated to 85°C BEFORE placing the watch glass over the sample. Laboratory tests have proven that the addition of the ribbed watch glass will add approximately 10°C to the sample temperature, bringing the sample temperature up to 95°C. Refer to page 7 of the operations manual for instructions on HotBlock™ temperature adjustment.

3.3 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool.

3.4 After cooling, dilute samples to 50mL with DI Water.

3.5 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

Note: The ltration step should be performed slowly with little pressure placed on the

plunger. If excessive back pressure occurs, stop ltration and allow sediments to “settle out”. Applying pressure to the plunger may cause sample “blow through” allowing sediment to pass through the lter into the digestate.

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HotBlock™: Operation and Instruction Manual EPA Method 200.2, Revision 2.8

4.0 Procedure, Solids Sample Preparation

4.1 Sieve a dried sample using a 5-mesh polypropylene sieve and grind in a mortar and pestle. Weigh a representative sample of 0.5 ±0.01g into a digestion vessel.

4.2 Add 2mL of (1+1) HNO3 and 5mL of (1+4) HCl+DI. Cover with a ribbed watch glass (SC505) or reux cap (SC506),and place in the HotBlock™ at 95°C. Refer to page 7 of the operations manual for instructions on

HotBlock™ temperature adjustment.

4.3 Heat sample for 30 minutes.

4.4 (Optional) Although step 3 is the nal heating step for EPA Method 200.2, if the sample is suspected of having a high concentration of organic compounds, it is recommend to complete this step:

Add 2mL of 30% H2O2 to the well-cooled sample. Allow the exothermic

reaction to occur (approximately 10 minutes) and place the sample back in the HotBlock™ at a temperature of 10° less than the original set point for an additional 30 minutes. The reaction with the H2O2 raises the sample temperature. Boiling should not occur if the temperature of the HotBlock™ is lowered.

Note: H2O2 helps aid in the breakdown of high organic compounds in the sample thus

creating a more complete digestion.

4.5 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool completely.

4.6 Bring sample volume to 50mL with DI water.

4.7 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

Note: The ltration step should be performed slowly with little pressure placed on the

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Method 200.2. Safety concerns are also part of the full method. Follow the instructions listed in EPA Method 200.2. These steps should only be used as a guide to help improve the performance of your HotBlock™.

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HotBlock™: Operation and Instruction Manual EPA Method 200.7, Revision 4.4

Adaptation for EPA Method 200.7, Revision 4.4 for use with the Environmental Express HotBlock™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA digestion procedure 200.7 for use with the Environmental Express HotBlock™. EPA Method 200.7 is for the determination of total recoverable analytes in groundwater, surface water, drinking water, wastewater, and (with the exception of silica) in solid samples such as sediment, sludge and soil. Use EPA Method 200.7 for reference while following the sample preparation steps outlined below. A complete list of elements appropriate for analysis is included in EPA Method 200.7. Analysis can be performed by ICP.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Number SC100, SC150*, or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

2.4 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

*Note: For all procedures, when using the SC150 block with the SC490 digestion vials with

a 100mL sample, double the volume of all reagents and acids added.

3.0 Procedure, Total Recoverable Elements, Aqueous Sample (EPA Method 200.7, Paragraph 11.2)

3.2 Add 1mL 1:1 HNO3 and 0.5mL 1:1 HCl and swirl. Heat in the HotBlock™ at a sample temperature of 85°C and evaporate to about 10mL taking care that the cup does not go dry. This will take approximately 2 hours.

3.3 Cover the vessel with a disposable watch glass (catalog # SC505) and reux an additional 30 minutes.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

that a 50mL, 5% acid solution is heated to 85°C BEFORE placing the watch glass over the sample. Laboratory tests have proven that the addition of the ribbed watch glass will add approximately 10°C to the sample temperature, bringing the sample temperature up to 95°C. Refer to page 7 of the operations manual for instructions on HotBlock™ temperature adjustment.

3.4 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool. Bring samples up to volume with DI water.

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HotBlock™: Operation and Instruction Manual EPA Method 200.7, Revision 4.4

3.5 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

Note: The ltration step should be performed slowly with little pressure placed on the

plunger. If excessive back pressure occurs stop ltration and allow sediments to “settle out”. Applying pressure to the plunger may cause sample “blow through” allowing sediment to pass through the lter into the digestate.

4.0 Procedure, Total Recoverable Elements, Solids Sample (EPA Method 200.7, Paragraph 11.3)

4.1 For each digestion procedure, transfer 0.5g ± 0.01g of a dried sieved sample into the SC475 polypropylene vessel.

4.2 Add 2.0mL (1:1) HNO3 and 5mL (1:4) HCl and swirl. Cover the vessel with a disposable watch glass (catalog # SC505) and reux an additional 30 minutes at a sample temperature of 85°C.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

4.3 Allow to cool and bring to 50mL volume with DI water.

4.4 Filter with SC0401 (or appropriate FilterMate) to remove insoluble material.

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Method 200.7. Safety concerns are also part of the full method. Follow the instructions listed in EPA Method 200.7. These steps should only be used as a guide to help improve the performance of your HotBlock™.

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HotBlock™: Operation and Instruction Manual EPA Method 200.8

Adaptation for EPA Method 200.8, for use with the Environmental Express HotBlock™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA digestion procedure 200.8 for use with the Environmental Express HotBlock™. EPA Method 200.8 is for the determination of total recoverable analytes in groundwater, surface water, drinking water, wastewater, and (with the exception of silica) in solid samples such as sediment, sludge and soil. Use EPA Method 200.8 for reference while following the sample preparation steps outlined below. A complete list of elements appropriate for analysis is included in EPA Method 200.8. Analysis can be performed by ICP-MS.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Numbers SC100, SC150*, or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

2.4 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

*Note: For all procedures, when using the SC150 block with the SC490 digestion vials with

a 100mL sample, double the volume of all reagents and acids added.

3.0 Procedure, Aqueous Sample Preparation -- Dissolved Analytes (EPA Method 200.8, Paragraph 11.1)

3.1 For the determination of dissolved analytes in ground and surface waters, pipet a 20mL or greater aliquot of ltered, acid-preserved sample into the SC475 digestion vessel.

3.2 Add an appropriate volume of (1+1) HNO3 to adjust the acid concentration of the aliquot to approximate a 1% (v/v) nitric acid solution. If the direct addition procedure is being used, add internal standards, cap and mix.

Note: If a precipitate is formed during acidication, transport or storage the sample

aliquot must be treated using procedures for Total Recoverable Analytes.

4.0 Procedure, Aqueous Sample Preparation — Total Recoverable Analytes (EPA Method 200.8, Paragraph 11.2)

Note: This section applies to water samples containing turbidity of greater than 1 NTU.

4.1 For each digestion procedure, transfer 50mL of well-mixed, unltered, acid-preserved sample into the SC475 polypropylene vessel.

4.2 Add 1.0mL (1+1) HNO3 and 0.5mL of (1+1) HCl and swirl. Heat in the HotBlock™ at a sample temperature of 85°C. The HotBlock™ set temperature should be approximately 105°C. The temperature of a reference blank should be tested to ensure correct temperature.

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HotBlock™: Operation and Instruction Manual EPA Method 200.8

4.3 Reduce the volume of the sample aliquot to about 10mL at this temperature. This should take about 2.5 hours.

4.4 Place a ribbed watch glass (SC505) over the digestion vessel to reduce additional evaporation.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

4.5 Gently reux the sample for 30 minutes.

4.6 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool.

4.7 Add reagent water to bring the sample to the 50mL mark on the digestion vessel. Cap and mix.

4.8 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

Note: The ltration step should be performed slowly with little pressure placed on the

plunger. If excessive back pressure occurs, stop ltration and allow sediments to “settle out.” Applying pressure to the plunger may cause sample “blow through” allowing sediment to pass through the lter into the digestate.

4.9 Prior to analysis, adjust the chloride concentration by pipetting 20mL of the prepared solution into another SC475 digestion vessel and bring up to 50mL volume with reagent water. If the dissolved solids in this solution are >0.2%, additional dilution may be necessary to prevent clogging of the extraction and/or skimmer cones. Note the dilution factor for concentration calculations. If the direct addition procedure is being used, add internal standards, cap and mix.

5.0 Procedure, Solid Sample Preparation

5.1 For each digestion procedure, transfer 0.5g ± 0.01g of a dried sieved sample into the SC475 polypropylene vessel.

5.2 Add 2.0mL (1:1) HNO3 and 5mL (1:4) HCl and swirl. Cover the vessel with a disposable watch glass (catalog # SC505) and reux an additional 30 minutes at a sample temperature of 85°C.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

5.3 Allow to cool and bring to 50mL volume with DI water.

5.4 Filter with SC0401 (or appropriate FilterMate) to remove insoluble material.

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Method 200.8. Safety concerns are also part of the full method. Follow the instructions listed in EPA Method 200.8. These steps should only be used as a guide to help improve the performance of your HotBlock™.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Methods 245.1, 7470, 7471

Adaptation of EPA Methods for Mercury Digestions 245.1, 7470, 7471, for use with the Environmental Express HotBlock™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA Digestion Methods 245.1, 7470 and 7471 for use with the Environmental Express HotBlock™. EPA Methods 245.1 and 7470 are for the determination of mercury in aqueous samples and TCLP extracts. EPA Method 7471 is for the determination of mercury in soil, oil and sediment. Use the full EPA Methods for reference while following the sample preparation steps outlined below.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Numbers SC100, SC150*, or SC154

2. Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

3. Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

*Note: For all procedures, when using the SC150 block with the SC490 digestion vials with

a 100mL sample, double the volume of all reagents and acids added.

3.0 Procedure, Aqueous Sample Preparation

3.1 Add 20mL of well-mixed sample to a SC475 digestion vessel or 2mL of TCLP extract and 18mL water.

Note: This is a 10x dilution for instruments that can achieve the detection limit including

the dilution, otherwise digest 20mL of TCLP extract.

3.2 Add 20mL of standard solutions or appropriate amount of standard spiking solution to give desired concentration when diluted to 20mL.

3.3 Add 0.5mL of concentrated HNO3.

3.4 Add 1.0mL of concentrated H2SO4.

3.5 Mix thoroughly. Add 3mL of 5% KMnO4 and let stand for 15 minutes. If sample does not maintain purple or brown color, add additional portions to all samples, blanks and standards until the color persists for at least 15 minutes.

3.6 Add 1.6mL of 5% persulfate solution. Place watch glass or reux cap on top of digestion vessel to allow pressure to vent while minimizing evaporative loss.

3.7 Digest the sample for 2 hours at 95°C.

3.8 Remove samples and let cool to room temperature.

3.9 Add 1.2mL of sodium chloride/hydroxyl amine hydrochloride solution.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Methods 245.1, 7470, 7471

4.0 Procedure, Soil, Oil and Sediments, 7471A:

4.1 Weigh 0.25-0.30g of homogenized sample into a tube. For best results, weigh the sample directly in the vessel on a tared balance.

4.2 Add 5mL DI water and 5mL aqua regia.

4.3 Heat for 2 minutes at 95 ±3°C.

4.4 Allow samples to cool and add 25mL DI water.

4.5 Add 7.5mL of KMnO4 and let stand for 15 minutes. If sample does not maintain purple or brown color, add additional portions to all samples, blanks and standards until the color persists for at least 15 minutes. Heat samples at 95 ±3°C for 30 minutes.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

that a 50mL sample is heated to 85°C BEFORE placing the watch glass over the sample. Laboratory tests have proven that the addition of the ribbed watch glass will add 10°C to the sample temperature, bringing the sample temperature up to 95°C. Refer to page 7 of the operations manual for instructions on HotBlock™ temperature adjustment.

4.6 Let samples cool to room temperature and add 3mL of Sodium Choloride-Hydroxylamine Sulfate solution.

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Methods 245.1, 7470 and 7471. Safety concerns are also part of the EPA Methods. These steps should only be used as a guide to help improve the performance of your HotBlock™.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Method 365.2

Adaptation of EPA Method 365.1, Determination of Phosphorous by Semi-Automated Colorimetry, for use with the Environmental Express HotBlock™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA Method 3651 for use with the Environmental Express HotBlock™. EPA Method

365.1 is for the determination of phosphorous in drinking water, surface water and saline water and in domestic and industrial wastes. Use EPA Method 365.1 for reference while following the sample preparation steps outlined below. Range is 0.01 to 0.5 mg/L.

2.0 Apparatus and Materials

2.1 HotBlock™ for metals digestions — Model Numbers SC100, SC150*, or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

* Note: For all procedures, when using the SC150 block with the SC490 digestion vials

with a 100mL sample, double the volume of all reagents and acids added.

3.0 Procedure, Aqueous Sample Preparation

3.1 For each digestion procedure, transfer 50mL of sample (or appropriate volume for your lab) into the SC475 polypropylene vessel.

3.2 Add 1mL of H2SO4 solution and swirl. (11 N H2SO4 — Slowly add 310mL concentrated H2SO4 to 600mL distilled water. When cooled dilute to 1 liter.)

3.3 Add 0.4g of ammonium persulfate.

3.4 Heat the sample in the HotBlock™ at approximately 100°C for 40 minutes. The sample should slightly boil.

Note: Adjust the HotBlock™ temperature so that the sample obtains a temperature

of 100°C. Please refer to page 7 of the HotBlock™ Operation Manual for temperature adjustment and principles of operation.

3.5 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool.

3.6 After cooling, dilute to 50mL with DI Water.

3.7 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

Note: The ltration step should be performed slowly with little pressure placed on the

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Method 365.1. Safety concerns are also part of the full method. Follow the instructions listed in EPA Method 365.1. These steps should only be used as a guide to help improve the performance of your HotBlock™.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Method 3050B

Adaptation of EPA Method 3050B for use with the Environmental Express HotBlock™™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA Method 3050B for use with the Environmental Express HotBlock™. EPA Method 3050B is for the preparation of sediment, sludge, and soil samples for analysis. Use EPA Method 3050B for reference while following the sample preparation steps outlined below. A complete list of elements appropriate for analysis is included in EPA Method 3050B. Analysis can be performed by ame atomic absorption, GF/AA, ICP and ICP-MS.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Numbers SC100, SC150*, or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

2.4 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

* Note: When using the SC150 block with the SC490 digestion vials with a 100mL sample,

double the volume of all reagents and acids added.

3.0 Procedure, Sample Preparation

3.1 Mix sample thoroughly to achieve homogeneity and sieve if appropriate. For each digestion procedure, weigh to the nearest 0.01 gram and transfer a 0.5-1-gram aliquot (or appropriate amount for your lab) to the SC475 polypropylene digestion vessel. For best results, weigh the sample directly in the vessel on a tared balance.

3.2 Add 5mL (1:1) HNO3 + DI Water and swirl. Cover with a ribbed watch glass or reux cap and heat the sample in the HotBlock™ at 95±5°C for 15 minutes without boiling.

Note: If using the watch glass, adjust the HotBlock™ temperature so that a 50mL, 5% acid

solution is heated to 85°C. Laboratory tests have proven that the addition of the ribbed watch glass will add approximately 10°C to the sample temperature. Refer to page 7 of the operations manual for instructions on HotBlock™ temperature adjustment.

3.3 Allow the sample to cool, then add 2.5mL concentrated HNO3 and reux at 95°C for 30 minutes. Repeat this step until NO brown fumes are given off by the sample.

3.4 Heat sample with the ribbed watch glass to a volume of about 5mL or for 2 hours at 95±5°C . Do not allow the sample to boil or go dry. Neither of these aspects should occur if the temperature of the HotBlock™ is adjusted correctly.

3.5 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and cool completely (it is very important that samples are cooled completely).

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Method 3050B

3.6 Add 1mL DI Water and 1.5mL of 30% H2O2 slowly. Allow an exothermic reaction to occur. Wait 5-10 minutes and place samples back in the HotBlock™ with the ribbed watch glasses in place. If effervescence starts to occur lift the samples out of the HotBlock™ and allow the reaction to continue. Do not let the samples foam out of the vessel. (Reducing the HotBlock™ display temperature by 10°C should reduce the effervescence while maintaining the sample temperature).

3.7 Continue to add 0.5mL of H2O2 (no more than 5mL total) until the sample remains unchanged in color (no longer than 30 minutes). Continue heating for a total of 2 hours or until volume has been reduced to approximately 5mL.

3.8 For the analysis of samples for FLAA or ICP-AES, add 5mL concentrated HCl to each sample and cover with a ribbed watch glass and reux at 95°C for 15 minutes. GFAA and ICP-MS digestions, skip this step.

3.9 After cooling, dilute to 50mL with DI Water.

3.10 If necessary, lter with SC0401 (or appropriate FilterMate) to remove insoluble material.

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in EPA Method 3050B. Safety concerns are also part of the full method. Follow the instructions listed in EPA Method 3050B. These steps should only be used as a guide to help improve the performance of your HotBlock™.

Adaptation of NIOSH Method 7303 for use with the Environmental Express HotBlock™™ Digestion System Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to NIOSH Method 7303 for use with the Environmental Express HotBlock™. Method 7303 is for the preparation of cellulose ester membrane lters commonly used in air sampling devices. Use EPA Method 7303 for reference while following the sample preparation steps outlined below. A complete list of elements appropriate for analysis is included in Method 7303. Analysis can be performed by ICP or AA.

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Numbers SC100, SC150*, or SC154

2.2 Polypropylene Digestion Vessels — Catalog # SC475 (or SC490 for use with HotBlock™ SC150)

2.3 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610 )

2.4 FilterMate™ — Catalog # SC0401 (or appropriate FilterMate) for sample ltration if necessary

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HotBlock™: Operation and Instruction Manual NIOSH Method 7303

* Note: When using the SC150 block with the SC490 digestion vials with a 100mL sample,

double the volume of all reagents and acids added.

3.0 Procedure, Filter Preparation

3.1 Remove lter from cassette holder and fold into quarters taking care not to lose any sample.

3.2 Place in SC475 digestion vessel and add 1.25mL HCl.

3.3 Cover with plastic watch glass or reux cap. Place in HotBlock™ and heat at a sample temperature of 95°C for 15 minutes.

Note: If using the watch glass, adjust the HotBlock™ temperature so that a 50mL, 5% acid

3.4 Remove samples from the HotBlock™ and cool for 5 minutes.

3.5 Remove watch glass and add 1.25mL HNO3. Replace watch glass and return to HotBlock™ at sample temperature of 95°C for 15 minutes.

3.6 Remove the sample from the HotBlock™ and cool for at least 5 minutes. Rinse watch glass into vessel. Discard watch glass.

3.7 Dilute to 25mL nal volume with distilled, deionized type II water.

All QC samples, concentration limitations, elemental lists and reagent specications are addressed in depth in Method 7303. Safety concerns are also part of the full method. Follow the instructions listed in Method 7303. These steps should only be used as a guide to help improve the performance of your HotBlock™.

Sample Preparation for Lead Analysis with the GhostWipe

Revised 05.05

Methodology Note:

The following procedure has been written as an aid for use with the Environmental Express HotBlock™™ and strictly follows HUD (Housing and Urban Development) guidelines for Lead in Dust Wipes Appendix A-5.0 which references NIOSH 7082.

1.0 Scope and Application

1.1 This application deals with the preparation of samples using lead wipes, specically the GhostWipe from Environmental Express. The sample is heated in the presence of Nitric and Hydrochloric acids to dissolve the wipe and all lead compounds into solution. Analysis can be performed by ame atomic absorption (FLAA) or inductively coupled plasma technique (ICP).

2.0 Apparatus and Materials

2.1 HotBlock™ for Metals Digestions — Model Numbers SC100, SC150*, or SC154

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HotBlock™: Operation and Instruction Manual Using the GhostWipe

2.2 Ghost Wipe — Catalog # SC4210 or SC4250

2.3 Polypropylene Digestion Vessels — Catalog # SC475 (SC490 for HotBlock™ SC150)

2.4 Ribbed Watch Glasses, Catalog # SC505 or Reux Caps, Catalog # SC506 (for use with SC490 vials for HotBlock™ SC150, use Ribbed Watch Glasses, Catalog # SC610)

2.5 FilterMate™ — optional if sample does not completely dissolve

* Note: For all procedures, when using the SC150 block with the SC490 digestion vials

with a 100mL sample, double the volume of all reagents and acids added.

3.0 Reagents

3.1 Concentrated Reagent-grade HNO3 (5mL repipet dispenser recommended)

3.2 Concentrated Reagent-grade HCl (5mL repipet dispenser recommended)

4.0 Procedure

4.1 Transfer the wipe to the SC475 digestion cup. It is recommended that the wipe is sent to the sampling area with a cup and wipe so no transfer steps are required. The wipe must be transported in a rigid-walled container according to the sampling procedure ASTM E1728.

4.2 Add 10mL DI Water, 2mL HNO3 and 2mL HCl. Cover with a ribbed watch glass.

4.3 Heat the sample for 45 minutes at 95°C.

Note: When using a watch glass, adjust the set point temperature of the HotBlock™ so

that a 50mL solution is heated to 85°C BEFORE placing the watch glass over the sample. Laboratory tests have proven that the addition of the ribbed watch glass will add approximately 10°C to the sample temperature, bringing the sample temperature up to 95°C. Refer to page 7 of the operations manual for instructions on HotBlock™ temperature adjustment.

4.4 Using the polycarbonate transfer racks, remove samples from the HotBlock™ and allow them to cool for approximately 10 minutes. Bring the sample to 50mL volume. If excess amounts of undigested material remain, lter the sample using a 2.0µm Teon® FilterMate.

4.5 Cap and mix well.

According to AIHA Policies 2001- Revision Nov. 2000, one LCS, one matrix spike and one duplicate must be run every 20 samples. “The LCS shall be a solid matrix material with an established concentration obtained from a source independent of the instrument calibration and traceable to NIST or other similar reference material. Liquid spikes may not be used for preparing LCSs”. Environmental Express does offer NIST traceable spiked Ghost Wipes. The catalog number is SC4252. The range is 175-200µg of Lead per wipe.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Method 3060

Adaptation of EPA Method 3060 for use with the HotBlock™™ and StirBase Systems Revised 05.05

1.0 Scope and Application

1.1 The following procedures have been written as an aid to EPA Method 3060A for use with the Environmental Express HotBlock™ and StirBase. EPA Method 3060A is an alkaline digestion procedure for extracting hexavalent chromium [Cr(6+)] from soluble, adsorbed, and precipitated forms of chromium compounds in soils, sludges, sediments, and similar waste materials. Use EPA Method 3060A for reference while following the sample preparation steps outlined below. The quantication of Cr6+ in Method 3060A digests should be performed using a suitable technique with appropriate accuracy and precision.

2.0 Apparatus and Materials

2.1 HotBlock™ for sample digestion – Model Numbers SC100, SC154, SC150, or SC151

2.2 StirBase stirring device – Catalog # SC160

2.3 Polypropylene Digestion Vessels – Catalog # SC475 (or SC490 for use with the SC150 or SC151 HotBlocks™)

2.4 Ribbed Watch Glasses – Catalog # SC505 (or SC610 for use with the SC150 or SC151 HotBlocks™)

2.5 Reux Caps – Catalog # SC506 (used as an alternative to the SC505 only)

2.6 Stir Bars – Catalog # SC168

2.7 FilterMate – Catalog # SC0407 (or appropriate FilterMate) for sample ltration if necessary

2.8 FlipMate – Catalog # SC0301 (or appropriate FlipMate) for sample ltration if necessary

3.0 Procedure, Solid Sample Preparation

3.1 Place 2.5 ±0.10 g of the eld-moist sample into a clean and labeled digestion vessel. The sample should have been mixed thoroughly before the aliquot is removed.

3.2 For the specic sample aliquot being spiked, the spike material should be added directly to the sample aliquot at this point.

3.3 Add 50mL±1mL of digestion solution to each sample using a graduated cylinder, and also add approximately 400 mg of magnesium chloride and 0.5mL of 1.0M phosphate buffer. For analytical techniques that can correct for oxidation/reduction of Cr, the addition of Mg(2+) is optional. Cover all samples with watch glasses or reux caps.

3.4 Stir the samples continuously (unheated) for at least ve minutes using the StirBase.

3.5 Heat the samples to 90 - 95ºC, then maintain the samples at 90 - 95ºC for at least 60 minutes with continuous stirring.

3.6 Gradually cool, with continued agitation, each vessel to room temperature.

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HotBlock™: Operation and Instruction Manual Adaptation of EPA Method 3060

3.7 Filter each sample using a 0.45µm FlipMate (SC0601).

3.8 Adjust the pH of the digestate accordingly to the method being used for analysis. If a precipitate forms, the sample should be ltered as in 3.7.

3.9 Adjust the sample volume to 100mL with reagent water. Mix well. The sample digestates are new ready to be analyzed.

All QC samples, concentration limitations, interferences, and reagent specications are addressed in depth in EPA method 3060A. Safety concerns are also part of the full method. Follow the instructions listed in EPA method 3060A. These steps should only be used as a guide to help improve the performance of your HotBlock™ and StirBase.

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HotBlock™: Operation and Instruction Manual 50mL HotBlock™ Accessories and Consumables

Accessories and Consumables for 50mL HotBlocks™

Polycarbonate Transfer Racks

Each sample transfer rack for the HotBlock™ is designed to hold and handle eighteen SC475 50mL digestion vessels. Racks are made of polycarbonate for heat and acid resistance and t over the HotBlock™ to facilitate handling of samples and improve temperature and evaporation uniformity.

Polycarbonate Transfer Rack Each Catalog # SC200

Plastic Storage Racks

24-cup capacity plastic racks neatly hold the SC475 digestion cup. Made of polypropylene, racks accommodate any tube up to 30mm and are stackable for efcient storage.

Plastic Storage Rack Each Catalog # SC446

Urethane Foam Storage Racks

Low-cost storage system uses high density urethane foam for semi-permanent storage of digested samples. Each rack holds 25 capped SC475 digestion cups. Racks with cups may be stacked to save space. Overall size of rack is 10" x 10" x 1".

Urethane Foam Storage Racks Pack of 5 Catalog # SC700

Temperature Probe

The temperature probe accessory allows the technician to monitor actual sample temperature in 50mL vessels. The digital thermometer is adjustable in Teon® holder to allow placement of thermometer tip just above bottom surface of digestion vessel. Thermometer has LCD display and can be set in either Fahrenheit or Celsius.

Description Quantity Catalog #

Temperature Probe (thermometer to 150ºC) Fits SC475 Each SC980

High Range Temperature Probe (thermometer to 250ºC) Fits cups SC432, SC545, and SC475 Each SC983

Digital Digestion Timer

Use of this digital timer with the HotBlock™ allows the analyst to turn the HotBlock™ on and off automatically. Digestions that are begun late in the work day may be completed and cooled while unattended. The timer plugs directly into standard wall outlet.

Digital Digestion Timer Each Catalog # SC305

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HotBlock™: Operation and Instruction Manual 50mL HotBlock™ Accessories and Consumables

Disposable Polypropylene Digestion Vessels

These carefully engineered digestion vessels provide premium performance in your HotBlock™™ or AutoBlock™. Molded of claried homopolymer polypropylene, these vessels provide a higher working temperature and greater chemical resistance than commonly used co-polymer polypropylene.

Each vessel is graduated to 50mL and has a total capacity of 68mL. Molded-in graduations are extremely accurate, allowing analysts to easily reproduce volumes to within 0.5%. Using the vessels’ graduations for sample measurement reduces the need for graduated cylinders and volumetric asks while eliminating sample transfers. The result is a “one-cup” system that greatly reduces labor and costs associated with metals preparation.

The 33mm threaded cap is lined with a 0.040" polyethylene-faced foam liner for a leak-proof seal. Only the metals-free polyethylene liner comes into contact with the sample. SC475 vessels come in cases of 500 and are packaged to ship as a standard size UPS package, keeping shipping costs at a minimum. Vessels come standard with green caps. Vessels with white caps are also available (SC480-W).

• Certied for low metals background

• Compact packaging reduces shipping costs

• Lined closure system ensures leak-free performance with no contamination

• Accurate graduations eliminate the need for graduated cylinders

Specialty Digestion Vessels are also available for a variety of specialty applications. Visit our web site at www.envexp.com or call us for more information.

Disposable 50mL Digestion Cup Pack of 500 Catalog # SC475

Ribbed Watch Glasses

44mm ribbed watch glasses t all 50mL digestion vessels. Disposable polypropylene construction is naturally free of contaminants. Ribbed design allows partial reux during digestion. Watch glass has a center stem to aid in handling.

Ribbed Watch Glasses, 44mm Pack of 1000 Catalog # SC505

Reux Cap

Special cap has a 0.5" hole in its center to allow the addition of reagents while cap remains in place on the SC475 digestion vessel. The disposable reux cap does not have to be removed during the digestion process. The cap is not ribbed, but ts over the top of the SC475 digestion vessel to maintain a centered position. Tests have shown equal reux between SC506 reux cap and SC505 watch glass.

Reux Cap for SC475 Pack of 1000 Catalog # SC506

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HotBlock™: Operation and Instruction Manual 100mL HotBlock™ Accessories and Consumables

Accessories and Consumables for 100mL HotBlocks™

Polycarbonate Transfer Racks

This set of two polycarbonate racks was designed to t the SC150 Hot Block (see photo page 4). A 15-place rack paired with a 10-place rack give you 25 sample capacity. Racks t the SC150 HotBlock™ securely for safe, accurate digestions.

Polycarbonate Tramsfer Racks for SC150 HotBlock™ Set of 2 Catalog # SC225

Wire Storage Rack for SC490s

Powder-coated wire rack shown above is for storing SC490 cups. Rack has an 18-cup capacity.

Wire Storage Rack Each Catalog # SC7150

Temperature Probe

This temperature probe ts SC490 cups and allows the analyst to monitor actual temperature in a 100mL sample. The digital thermometer is adjustable in a Teon® holder to allow placement of the thermometer tip in desired position in cup. Thermometer has LCD display and may be read in either Fahrenheit or Celsius.

Temperature Probe (thermometer to 150ºC) for SC490 Each Catalog # SC981

Disposable Polypropylene Digestion Vessels for use with SC150 HotBlock™

This 125mL, wide-mouth digestion vessel is supplied with a 48mm screw cap. The cap is lined with coextruded polyethylene foam for leak-proof performance. Made of homopolymer polypropylene, the SC490 digestion vessel is designed for use in the SC150 HotBlock™. Vessels are graduated at 10mL, 25mL and 50mL, 75mL and 100mL.

Disposable 125mL Digestion Cup Pack of 225 Catalog # SC490

Ribbed Watch Glass

52mm ribbed watch glass is designed for use with SC490, 125mL digestion vessel. The disposable polypropylene watch glass has a stem in its center to aid in handling.

Ribbed Watch Glass, 52mm Pack of 500 Catalog # SC610

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HotBlock™: Operation and Instruction Manual 15mL HotBlock™ Accessories and Consumables

Accessories and Consumables for 15mL HotBlocks™

Polycarbonate Transfer Rack

These polycarbonate racks t the SC196 HotBlock™. The racks hold our SC415 digestion vessels securely, assisting the analyst in performing safe, accurate digestions. Three 32-place racks give you 96-sample capacity.

Polycarbonate Tramsfer Racks for SC196 HotBlock™ Set of 3 Catalog # SC296

Temperature Probe

This temperature probe ts SC415 cups and allows the analyst to monitor actual temperature in a 15mL sample. The digital thermometer is adjustable in a Teon® holder to allow placement of the thermometer tip in desired position in cup. Thermometer has LCD display and may be read in either Fahrenheit or Celsius.

Temperature Probe (thermometer to 150ºC) for SC415 Each Catalog # SC985

Polypropylene Digestion Vessels for use with SC196 HotBlock™

These screw cap digestion vessels for 15mL samples, have a total volume of 18mL. Molded-in graduations are in 5mL increments up to 15mL.

Disposable 15mL Digestion Cups with Caps Pack of 1,000 Catalog # SC415

Ribbed Watch Glass

19.5mm ribbed watch glass is designed for use with SC415, 15mL digestion vessel. The disposable polypropylene watch glass has a stem in its center to aid in handling.

Ribbed Watch Glass, 19.5mm Pack of 1000 Catalog # SC417

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HotBlock™: Operation and Instruction Manual AirLite HEPA-Filtered Enclosure

AirLite™ HEPA-Filtered Enclosure

SC801:

Size: 25.5"h X 32"w X 24"d

Door Opening Size: 32"w x 17"h

Materials: Acrylic walls and door, Kydex® top and bottom plates

Fan: 117CFM, PVC Coated

Electrical: 120VAC, 1 amp, 3-Prong Plug

This bench-top enclosure for the HotBlock™ provides HEPA-ltered air for cleaner, more uniform digestions. The AirLite uses a quiet 117 CFM internal PVC coated fan that is easily accessible by the technician. The cabinet of the AirLite is constructed from PET-G for exceptional clarity. The door of the hood opens a full 180° to allow unrestricted access to the

chamber. The body of the enclosure rests in a thermoformed Kydex® bottom that traps spills and can easily be removed for cleaning.

The AirLite is designed to enhance the use of the HotBlock™, and can reduce sample contamination during the digestion process. The HEPA lter can be changed in minutes. The AirLite can be used anywhere a clean environment is required. It can be exhausted with standard 4" exible duct to the outside or into existing ductwork. Spare 117CFM fan included.

Description Catalog #

AirLite Enclosure SC801

Replacement HEPA Filter SC840

Replacement Exhaust Fan SC830

FlipMate™ Filtration Assemblies

The FlipMate offers a quick and effective method of ltering up to 125mL of sample. The device accepts two threaded digestion cups (cups are sold separately)

- one containing the sample to be ltered and an empty cup to receive the ltrate. The assembly is then “ipped” over and vacuum is applied. The sample is pulled through the lter into the empty cup. The ltered sample can then be capped and stored for later analysis. FlipMate is available with a variety of lters installed.

Description Sample Size Filter Material Porosity Quantity Catalog #

FlipMate 50 50mL PES Filter with Prelter 0.45µm 100 SC0601

FlipMate 50 50mL Glass Fiber 1.5µm 100 SC0602

FlipMate 100 100mL PES Filter with Prelter 0.45µm 50 SC0301

FlipMate 100 100mL Glass Fiber 1.5µm 50 SC0302

FlipMate 100 100mL PES with Prelter 0.2µm 50 SC0303

FlipMate 100 100mL Acid Washed Glass Fiber 0.7µm 50 SC0304

FlipMate 100 100mL Acid Washed Filter >10µm 50 SC0306

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HotBlock™: Operation and Instruction Manual Sample Filtration Supplies

FilterMate™ Filtration Systems

Dirty or particulate-laden samples may require that the digested sample be ltered prior to analysis. This is especially true with sludge, wastewater and soil samples.

FilterMate Systems provide a convenient and inexpensive method of ltration that requires no transfer steps. The FilterMate ts directly into the digestion cup and is pushed through the liquid being ltered to the bottom of the cup with a detachable plunger. After the ltration is complete, the plunger is removed and discarded while the lter assembly remains in the bottom of the cup.

This arrangement does not interfere with storage or use of the cup in an autosampler. FilterMates are available with different choices of lters.

Membrane Type Membrane Characteristics Sample Lot Applications Size Porosity Certied Quantity Catalog #

Membrane Type: Teon-faced Polypropylene Characteristics: Highest dirt capacity Applications: Most laboratory applications 50mL 2µm No 100 SC0401

Membrane Type: Acid-washed Glass Fiber Filter Characteristics: Porous Polyethylene Frit Applications: TCLP Extractions 50mL 0.7µm No 100 SC0404

Membrane Type: Teon w/additional Teon Prelter Characteristics: Not for particulate-laden samples Applications: Dissolved metals only 50mL 0.45µm No 100 SC0407

Membrane Type: Teon Characteristics: High dirt capacity Applications: Suitable for trace level analysis 50mL 2µm Yes 100 SC0408

Membrane Type: Teon Characteristics: Low solids Applications: Dissolved metals only 50mL 0.45µm Yes 100 SC0409

Membrane Type: Polyethylene Frit Characteristics: For use with SC415 15mL 2µm No 100 SC0421

Cup Holder for FilterMate Filtrations

This machined HDPE xture adds stability when performing FilterMate ltrations. Digestion cup is placed into center hole of FilterMate Holder prior to beginning ltration. The holder secures the digestion cup as the FilterMate is depressed through the liquid sample. SC0510

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HotBlock™: Operation and Instruction Manual GhostWipes for Surface Sampling

Take a sample with

GhostWipe.

Digest as usual in acid

solution.

GhostWipe™ For Surface Sampling, Including Lead and Beryllium Testing

This revolutionary product eases sample preparation and analysis of surface lead or surface dust. The GhostWipe is a sturdy wiping material moistened with DI water that holds together even on the roughest wiping surfaces. In the lab, the GhostWipe readily and completely dissolves during the digestion process. This feature provides more complete dispersion of analytes and more uniform recoveries.

In addition, there is no messy brous material to clog sample uptake capillary or nebulizer. GhostWipes meet all ASTM Designation E 1792 specications for sampling materials for lead in surface dust. Wipes are 15cm x 15cm and are supplied in individual sealed packets.

Ghost wipes totally

dissolve during digestion

for easy analysis.

Description Quantity Catalog #

GhostWipes 500 SC4210

GhostWipes 1,000 SC4250

Dust Sampling Template, 10cm x 10cm 250 C1010

Dust Sampling Template, 12" x 12" 100 C1012

Lead Wipe Standard in Screw-Cap, Rigid-walled Cup (SC475)

The lead wipe standard is a Ghost Wipe spiked with in-situ dust. Using an NISTtraceable solid sample, known amounts of lead are placed on a wipe and each sample is individually labeled with the exact amount of lead the wipe contains. Each spike sample contains 175-250 micrograms of lead per wipe and comes with a certicate of analysis showing the Sample ID# and the starting concentration of the dust.

Lead Wipe Standard with Cup Box of 10 Catalog # SC4252

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Environmental Express CURRENT User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual