Instruction Manual for Acid Digestion Vessels

Designers & Manufacturers

High Pressure Lab-Autoclaves, Pressure Leaf filters & sparkler Filter Press

(An ISO-9001 Certified Company)

6, PARMAR INDUSTRIAL ESTATE, BEL BAZAR, KURLA (W), MUMBAI 400 070. INDIA.

Tel. : (91) 22 2512 9273 / 6755 3029 / 28 Fax:- : (91) - 22 2510 95 65 Email :- amarequip@ amarequip.com Website :- http:///www.amarequip.com

MANUAL/Manual Acid Digestion Vessels

Page 1 of 10

INDEX
SR. NO. 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 PARTICULARS INSTALLATION OF AUTOCLAVE SAFETY PRECAUTIONS BEFORE STARTING WARRANTY CLAUSE SCOPE PREVENTIVE MAINTENANCE ASSUMPTION OF RISK NATURE OF PTFE POTENTIAL HAZARDS SAMPLE SELECTION PRESSURE & TEMPERATURE LIMITS OPERATING PROCEDURE SETTING UP THE VESSEL FOR USE TROUBLE SHOOTING & REMEDIES HYDROSTATIC TEST CERTIFICATE SUPPLIED SPARES LIST SPECIFICATION WORK SHEET PAGE NO. 3 3 3 4 4 5 5 6 7 8 9 10 10 11 12 13

MANUAL/Manual Acid Digestion Vessels

Page 2 of 10

1.0

INSTALLATION OF THE VESSEL:

We thank you very much for selecting an AMAR product & wish you all the very best to get the maximum out of our vessel. Kindly go through the manual thoroughly before using the vessel to ensure efficient & safe working with longer life. Also read the trouble shooting chapter & warranty clause carefully before making any call. First unpack the vessel completely (if packed in a wooden crate). The vessel is already in assembled condition. Fix the vessel position on a leveled surface. The vessel should be placed in a room with adequate & effective ventilation. It is preferable to have a hood with an exhaust fan over the vessel. This is the most effective arrangement to vent off any accidental leakage of hazardous gases. Any parts or equipment given separately should be bolted or mounted as instructed during the trials or read the respective headings in the manual.

2.0

SAFETY PRECAUTIONS BEFORE STARTING:

2.1 The area of operation should be well ventilated. 2.2 There should be no open flames in adjacent areas. 2.3 A continuous watch should be kept on reactions which are (i) Exothermic (ii) Involving highly reactive compounds such as Acetylene, Ethylene Oxide, Oxygen etc. (iii) dealing in flammable gases. 2.4 Chemicals of corrosive nature with material of construction of autoclave should not be used in this apparatus.

3.0

WARRANTY CLAUSE:
The apparatus is warranted for 12 months from the date of supply for any bad workmanship or any defective materials. The warranty does not include the parts that are subjected to constant wear due to running i.e, teflon beaker, rupture disc etc. However, if any damage is done to the equipment by (i) mishandling (ii) using corrosive chemicals (iii) carrying out explosive / out of control reactions (iv) failure due to non-compliance with the instructions mentioned in the manual. or (v) Any subsequent design modifications carried out without our permission. M/s. AMAR EQUIPMENTS PVT. LTD. will not be held responsible/liable for this damage or injuries. Parts / Material which are irreparable at site under

MANUAL/Manual Acid Digestion Vessels

Page 3 of 10

warranty may have to be sent at our works for repairs / replacement. Any free replacement if necessary shall be given only after inspection of the faulty part / material. NOTE : 1) Check the work order sheet enclosed to see the specification of vessel & optional accessories ordered & supplied to you. 2) Whenever the word optional is attached to any part or items, it means the item shall be provided only if ordered optionally. These items do not form part of standard equipment. 3) The specification & rating of the autoclave & material of construction : All the internal & external wetted parts of the autoclave shall be as per your purchase order, our specification work order sheet & our quotation unless specified. 4) P. No. : Part No. from drawing enclosed. 5) Refer nozzle orientation plan to locate the desired valve / nozzle.

4.0 SCOPE :
These instructions are to acquaint the user with the procedures to be followed and the precautions to be taken when using Acid Digestion Vessel, PTFE-lined digestion vessels provide a convenient means for dissolving analytical samples rapidly in strong acids or alkalis, it is important that the user understand the capabilities and limitations of the equipment and will be well aware of the safety precautions to be observed in its operation. The user should read these basic instructions carefully before starting to use any of these vessels It must be understood that the excellent mechanism for sample digestion and dissolution provided by these vessels can be hazardous if a vessel is misused. Therefore, careful reading and full compliance with these instructions must be observed in all applications.

5.0

PREVENTATIVE MAINTENANCE:
Periodic cleaning may be performed on the exterior surfaces of the instrument with a lightly dampened

cloth containing mild soap solution. There are no user serviceable parts inside the product other than what is specifically called out and discussed in this manual.

MANUAL/Manual Acid Digestion Vessels

Page 4 of 10

6.0

ASSUMPTION OF RISK:
Amar Equipment Pvt. Ltd. offers its PTFE-lined Acid Digestion Vessels to skilled analytical chemists

as an attractive means for digesting and dissolving analytical samples for analysis. Amar designed and manufactures these vessels to be as effective as possible when used within the limitations prescribed l. But, since the pressures generated within these vessels are solely dependent upon the nature of the materials being treated, the filling level and the amount of heat applied to promote the reaction, Amar will not be responsible for personal injuries or damage to the vessel, to the oven or to other equipment resulting from the use of these vessels. As with all laboratory operations, the user must assume responsibility for and institute safety procedures to protect all personnel from any hazards associated with this equipment. Rigid controls must be established to guarantee that the operator does not overcharge or overheat the vessel.

7.0

THE NATURE OF PTFE:

PTFE offers such unique inertness and high temperature usefulness that it is an obvious choice as

the material of construction for lining these acid digestion vessels. PTFE does, however, have two characteristics which make it somewhat less than perfect for this application, and the user who understands these deficiencies will be able to minimize the effect upon their work. First, PTFE has a tendency to creep or flow under pressure or load. This tendency is present even at room temperature and it is accentuated at higher temperatures. At operating temperatures above 150C the creep effect will become more pronounced, making it more difficult to maintain tight seals & resulting in deformation and shorter life for the PTFE components. The extent of the creep effect will be roughly proportional to the maximum operating temperature. Secondly, PTFE is a porous material. Although the materials and designs used in Amar Acid Digestion Vessels minimize the effects of this porosity, users of these vessels can expect to see evidence of vapor migration across the cover seal and through the wall of the liner itself. The thick walls and long path seals used in vessel liners also help to overcome these undesirable properties. Experiments have shown that the amount of solute lost in this manner during a normal digestion is negligible, but vapor migration will occur and frequently it will be sufficient to produce noticeable discoloration on the inner metal wall of the vessel body and the screw cap

MANUAL/Manual Acid Digestion Vessels

Page 5 of 10

8.0

POTENTIAL HAZARDS:
While many thousands of these vessels have been used safely and routinely for treating a great variety of

samples with different digestion media under a broad range of operating conditions, it is possible to create conditions under which these vessels will explode. The bulk of the reported incidents of this type have been caused by failure of the operator to recognize one or more of the following potential hazards. 8.1 Excessive temperature: - When a vessel is overheated, two factors come into play: (1) the vapor pressure of the materials in the vessel increases exponentially with temperature and (2) the strength of the materials from which the vessel is made falls off (again exponentially) if the vessel is heated above its maximum temperature limit. Dangerous overheating can be produced by ovens with defective temperature controls, by water baths boiling dry or by operator inattention or carelessness. 8.2 Excessive Pressure: - Excessive Pressure can be produced not only by overheating, as but also from uncontrolled gaseous reactions and from high pressure vapor pressure or explosive materials, otr from overloading the vessel.

8.3 Excessive loading: - When organic materials are treated in these vessels, they may liberate gases as
well as heat. Since the PTFE liner is an excellent thermal insulator, this internal heat will be translated into higher internal temperatures and pressures. The loading limits prescribed for these vessels are purposely conservative to ensure that the energy released from the sample will not over-stress the vessel. The user must also remember that when a water-based solution is heated to 250C it expands to fill a space approximately 25 percent larger than its volume at room temperature. If there is insufficient vapor space in the vessel to accommodate this expansion, the tremendous hydrostatic pressure which will be generated will destroy the vessel. 8.4 Explosive materials: - The nitro compounds produced when nitric acid reacts with certain organic materials may have explosive properties capable of destroying the vessel, even when present in quantities well within the normal recommended charging limits. Consider, for example, what might happen if nitroglycerin were produced by reactions in the vessel. For this reason, fats, fatty acids, glycerin and similar materials must not be treated with nitric acid in these vessels and cellulosic materials must not be treated with mixed nitric and sulfuric acids. Similarly, because of its unpredictable nature, perchloric acid must not be used in these vessels.

MANUAL/Manual Acid Digestion Vessels

Page 6 of 10

9.0

SAMPLE SELECTION

9.1 Inorganic materials: - Most inorganic digestions proceed smoothly without unusual hazards, using not more than 0.5 grams in the 100 ml vessel size. As in all reactions, the vessel must never be completely filled as there must always be vapor space above the surface of the charge. To be sure that there is adequate free space, the total volume of the charge must never exceed two thirds (66%) of the capacity of the cup when working with inorganic materials. By observing these limits and taking precautions to prevent overheating, there should be no unusual hazards in treating inorganic samples with mineral acids. Ores, rock samples, glass and other inorganic materials can be dissolved in acid digestion vessels using
2 strong mineral acids: HF, HCl, H SO, HNO, Aqua Regia and others. Digestion times for these materials can vary

anywhere from 2 hours to several days. Ordinary glass materials (SiO) will mandate the use of HF, sometimes in combination with HCl, or aqua regia. Temperatures in the range of 100 to 150C are routinely used. Alumina is routinely digested using 10% sulfuric acid. Temperatures used for these samples are typically in excess of 200C. It is advantageous, from the standpoint of minimizing the digestion time, to reduce the sample to granular or powder form prior to digestion. The increase in surface area of the sample has a significant impact on the reaction with the digestion aid. 9.2 Organic materials: - Many organic materials can be treated satisfactorily in these digestion vessels but careful attention must be given to the nature of the sample and to possible explosive reactions with the digestion media. In all cases, the size of the sample and the amount of oxidant used must be carefully controlled. For nitric acid digestions (Carius decompositions) of organic compounds, the dry weight of organic matter must not exceed 0.5 gram in the 100 ml size. Notice that both minimum and maximum amounts of acid are specified. If the sample contains less than the specified maximum amount of dry organic matter, the amount of nitric acid must be reduced proportionately. As stated above, fats, fatty acids, glycerin and similar materials which form explosive compounds in an intermediate stage must not be treated with nitric acid in these vessels. Digestions involving other organic materials must also be handled cautiously since it is impossible to list all of the potentially dangerous combinations which might arise. For best protection, the user and their supervisor should study each reaction carefully before proceeding to use the digestion vessel or any other pressure vessel, asking such questions as: Is the reaction exothermic? What intermediate and final products might be produced and what will be their behavior?

MANUAL/Manual Acid Digestion Vessels

Page 7 of 10

When working with new or unfamiliar materials it is always advisable to run preliminary experiments using small samples and observing the behavior of the reactants carefully. Organic samples are typically treated with concentrated nitric acid. Nitric - sulfuric mixtures are not recommended for digesting organic samples due to the possibility of forming potentially unstable reaction products. Digestion with perchloric acid can be dangerous, for the same reason, and must not be used. Typical heating times range from 1 to 8 hours. Temperatures in the 150 to 200C range are generally quite effective.

10.0

PRESSURE AND TEMPERATURE LIMITS

Maximum working pressures for each acid digestion vessel as shown in work sheet and orders. Extreme

care must be exercised to ensure that pressures do not exceed these prescribed limits. The user must understand that in acid systems the solubility of gases as NO, HCL and SO will be reduced as the temperature rises, having the effect of adding non-condensable gas to the vapor phase in a closed vessel. As a result, the amount of acid present, the acid concentration and the free head space above the liquid will all have a bearing on the pressure developed in a closed vessel. Free head space must therefore be provided in all procedures, and the volume and concentration of the acid must be held to a minimum. Maximum operating temperatures for each acid digestion vessel are shown in the individual listings. But these limits must be used cautiously because, with certain acids, pressures higher than the allowable limit will be generated if the vessel is heated to the listed maximum temperature.

MANUAL/Manual Acid Digestion Vessels

Page 8 of 10

11.0

OPERATING PROCEDURE:-

Part No. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Body Bottom False Head Body Clamp Compression Ring Body Clamp Bolt Rupture Disc Beaker Cap Beaker Locking Plate

Item Name

Material S.S. 316 S.S. 316 S.S. 316 S.S. 316 EN 8 H.T. S.S. 316 PTFE PTFE S. S. 304

Qty. 1 No. 1 No. 1 No. 1 No. 1 No. 6 Nos. 1 No. 1 No. 1 No. 1 No.

MANUAL/Manual Acid Digestion Vessels

Page 9 of 10

12.0

SETTING UP THE VESSEL FOR USE

12.1 To open the Vessel: Loosen the clamp bolts (P. No. : 6) in criss cross fashion with spanner provided & then unlock the latches. Remove the two half sections of body clamp (P. No. : 4), the head (P. No. : 3) can be lifted out from the body (P. No. : 1). Remove teflon beaker cap (P. No. : 8). Place the head (P. No. : 3) Carefully on proper location. Charge the vessel as required. Do not fill more than 66% of the filling capacity. 12.2 Closing the vessel for operation: First examine whether all fittings and teflon beaker are in good condition and correct position. If body teflon cap has extruded into a thin edge around the inside and outside diameters, remove the extruded portion with a sharp knife. Tighten the clamp bolts in a criss-cross pattern. Always keep the vessel upright during assembly and closing operations. There must always be adequate free space above the charge in the Vessel. Place the vessel in a temperature controlled oven and follow the heating and cooling procedure after digestion, allow the vessel to cool to ambient temperature on an aluminum plate or a metal table top. It is not good practice to cool the vessel in cold water or in a freezer. The internal forces will sometimes distort the liner, making it difficult to remove the liner from the vessel body. Usually the liner can be dislodged by pressing the uncovered vessel against a brass.

13.0 TROUBLE SHOOTING & ITS REMEDIES:

SR. NO.

PROBLEM

CAUSE

SOLUTIONS

Leakage Problem 1. Leakage from body clamps Other Problems 1. Pitting / Corrosion of wetted parts Chemicals / Acids corrosive to MOC used Use special MOC suitable to those chemicals. Clamp bolt loose. Tighten them.

MANUAL/Manual Acid Digestion Vessels

Page 10 of 10