Experiment Report of Laboratory Organization Preparation of NH4OH 2M 25% Solution

Arranged by Group 6: 1. Astri Nurul H 2. Ciko Rolly 3. Fibri Erwan S 4. Nurul Aina Putri 5. Siti Masrifah 6. Aura (113194016) (1131940xx) (1131940xx) (1131940xx) (113194034) (xxxxxxxxx)

International Chemistry Education

STATE UNIVERSITY OF SURABAYA MATHEMATIC AND NATURAL SCIENCE FACULTY CHEMISTRY DEPARTMENT 2014

I. II. III. IV.

TITLE DATE OBJECTIVE BASIC THEORY

: Preparation of NH4OH 2M 25% Solution : Monday, February 24th 2014 : To prepare 250 mL NH4OH 2M 25% solution :

A. Material Safety Data Sheet (MSDS) of NH3 DESCRIPTION CHEMICAL NAME SYNONYMS FORMULA : Ammonia, Anhydrous : Ammonia : NH3

CHEMICAL FAMILY : Inorganic MOL. WT. COMPOSITION : 17.03(NH3) : 99+% Ammonia

STATEMENT OF HEALTH HAZARD HAZARD DESCRIPTION: Ammonia is an irritant and corrosive to the skin, eyes, respiratory tract and mucous membranes. May cause severe burns to the eyes, lungs and skin. Skin and respiratory related diseases could be aggravated by exposure

EMERGENCY TREATMENT EFFECTS OF OVEREXPOSURE: Eye: lacrimation, edema, or blindness may occur. Skin: irritation, corrosive burns, blister formation may result. Contact with liquid will freeze the tissue and produce a caustic burn. Inhalation: acute exposure may result in severe irritation of the respiratory tract, bronchospasm, edema or respiratory arrest. Ingestion: Symptoms similar to Inhalation. Lung irritation and pulmonary edema may occur. Extreme exposure may result in death from spasm, inflammation or edema. EMERGENCY AID: Eye: flush with copious amounts of water for 15 minutes. Eyelids should be held apart and away from eyeball for thorough rinsing. Skin: flush with copious amounts of water for 15 minutes while removing contaminated clothing and shoes. Exercise caution when removing contaminated

clothing as it may be frozen to the skin. Do not rub or apply ointment on affected area. Inhalation: remove to fresh air. Administer oxygen or artificial respiration if necessary. Ingestion: if conscious, give large amounts of water to drink or may drink orange juice or citrus to counteract ammonia. Do NOT induce vomiting. NOTE TO PHYSICIAN: Lung injury and pulmonary edema may appear as a delayed phenomenon. Supportive treatment with necessary ventilation actions, including oxygen, may warrant consideration.

PHYSICAL DATA BOILING PT: -33C (-28F) FREEZING PT: -78C (-108F) VAPOR PRESSURE: 10 atm @ 25.7C SOLUBILTY IN WATER: 89.9 g/100cc @ 0C 7.4 g/100cc @100C SPECIFIC GRAVITY (H2O=1): 0.682 @ 4C (39F) EVAPORATION RATE (Water=1): Faster than water PERCENT VOLATILE: 100% SURFACE TENSION: 23.4 Dynes/cm @ 11.1C APPEARANCE &ODOR: Colorless gas/liquid and pungent odor VAPOR DENSITY (AIR=1): 0.596 @ 0C (32F)

FIRE AND EXPLOSION HAZARD SPECIAL FIRE-FIGHTING PROCEDURES: Must wear protective clothing and a positive pressure SCBA. Stop source if possible. Cool fire exposed containers with water spray. Stay upwind and use water spray to knock down vapor and dilute. UNUSUAL FIRE AND EXPLOSION HAZARDS: Outdoors, ammonia is not generally a fire hazard. Indoors, in confined areas, ammonia may be a fire hazard, especially if oil and other combustible materials are present. If relief valves are inoperative, heat-exposed storage containers may become explosion hazards. Ammonia contact with chemicals such as mercury, chlorine, iodine, bromine, silver oxide, or hypochlorites can form explosive

compounds. Special hazards with chlorine to form chloramine gas, also a primary skin irritant and sensitizer. Combustion may form toxic nitrogen oxides.

CHEMICAL REACTIVITY STABILITY: Stable at room temperature. Ammonia will react exothermically with acids and water. CONDITIONS TO AVOID: Explosive or violent reactions can occur from mixing ammonia with halogens, strong oxidizers, strong mineral acids, Nitric Acid, Fluorine, Nitrogen Oxide, etc Sensitive explosive mixtures can form when mixed with air and hydrocarbons, Ethanol and Silver Nitrate, Chlorine, etc. Explosive products are formed by the reaction of ammonia with Silver Chloride, Silver Oxide, Bromine, Iodine, Gold, Mercury, Tellurium Halides, etc. Ammonia is incompatible or has hazardous reactions with Silver, Acetaldehyde, Acrolein, Boron, Halogens, Perchlorate, Chloric Acid, Chloric Monoxide, Chlorites, Nitrogen Tetroxide, Tin, Sulfur, etc. Ammonia has a corrosive reaction with galvanized surfaces, copper, brass, bronze, aluminum alloys, mercury, gold, and silver. This is a partial list of incompatibilities. HAZARDOUS DECOMPOSITION PRODUCTS: Hydrogen and nitrogen gases above 450C (842F). Decomposition temperatures may be lowered by contact with certain metals.

SPILL OR LEAK PROCEDURES STEPS TO BE TAKEN: Wear protective clothing and respiratory protection, see Protective Equipment. Stop source if possible. If exposure concerns are present, stay upwind and use water spray downwind of leak source to absorb ammonia gas and dilute. Contain diluted run-off from drains, sewers, water systems, etc CAUTION: ADDING WATER DIRECTLY TO LIQUID SPILLS WILL INCREASE VOLATILIZATION OF AMMONIA, THUS INCREASING POSSIBILITY OF EXPOSURE. WASTE DISPOSAL: Listed as a hazardous substance under CWA (40 CFR 1164.40 CFR 117.3 Reportable Quantity 100 lbs. OR 45.4kg) Classified as a

hazardous waste under RCRA (40 CFR 261.32 Corrosive # D002). Comply with all Federal, State and local regulations. Suitably diluted product may be applied to agricultural land as fertilizer. Keep spill from entering streams, lakes or any water systems.

SPECIAL PROTECTION AND PROCEDURES RESPIRATORY PROTECTION: MSHA/NIOSH approved respiratory

protection that consists of a full face gas mask and canisters effective for anhydrous ammonia that enable use for entry and escape in emergencies. Refer to 29 CFR 1910.134 for requirements and selection. A positive pressure SCBA is required for entry into ammonia atmospheres at or above 300 ppm. VENTILATION: Local exhaust sufficient to keep ammonia gas below Permissible Exposure Limits. PROTECTIVE EQUIPMENT: Splash-proof, chemical safety goggles, rubber gloves and boots should be worn to prevent contact. Face shield can be worn over the goggles as added protection. Respiratory protection and cotton work clothes are recommended. Refer to 29 CFR 1910.132 to 1910.136 for requirements. A positive pressure SCBA is required for entry into ammonia atmospheres at or above 300 ppm.

SPECIAL PRECAUTIONS STORAGE AND HANDLING: Store in a cool, well-ventilated area with containers tightly closed. OSHA 29 CFR 1910.111 prescribes handling and storage requirements for anhydrous ammonia as a hazardous material. WORK-PLACE PROTECTIVE EQUIPMENT: Protective equipment should be stored near, but outside of ammonia area. Water for first aid, such as an eyewash station and safety shower, is to be kept available in the immediate vicinity. See 29 CFR 1910.141 for workplace requirements. DISPOSAL: Ammonia is listed as a hazardous substance under FWPCA. It is classified as RCRA hazardous waste due to corrosivity, See WASTE DISPOSAL. PERSONAL: Use protective equipment as needed. Do not wear contact lenses. Avoid unnecessary exposure.

B. Material Safety Data Sheet (MSDS) of NH4OH Section 1: Chemical Product and Company Identification Product Name: Ammonium hydroxide Synonym: Aqueous Ammonia; Strong Ammonia Solution; Stronger Ammonia Water

Section 2: Composition Composition: Name Ammonia, anhydrous Water % by Weight 27-31 69-73

Section 3: Hazards Identification Potential Acute Health Effects: Very hazardous in case of skin contact (corrosive, irritant, permeator), of eye contact (irritant), of ingestion, . Non-corrosive to the eyes. Non-corrosive for lungs. Liquid or spray mist may produce tissue damage particularly on mucous membranes of eyes, mouth and respiratory tract. Skin contact may produce burns. Inhalation of the spray mist may produce severe irritation of respiratory tract, characterized by coughing, choking, or shortness of breath. Severe over-exposure can result in death. Inflammation of the eye is characterized by redness, watering, and itching. Skin inflammation is characterized by itching, scaling, reddening, or, occasionally, blistering. Potential Chronic Health Effects: CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS:

Mutagenic for bacteria and/or yeast. [Ammonia, anhydrous]. TERATOGENIC EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Not available. The substance is toxic to upper respiratory tract, skin, eyes. Repeated or prolonged exposure to the substance can produce target organs damage. Repeated or prolonged contact with spray mist may produce chronic eye irritation and severe skin irritation. Repeated or prolonged exposure to spray mist may produce respiratory tract irritation leading to frequent attacks of bronchial infection.

Repeated exposure to a highly toxic material may produce general deterioration of health by an accumulation in one or many human organs.

Section 4: First Aid Measures Eye Contact: Check for and remove any contact lenses. Immediately flush eyes with running water for at least 15 minutes, keeping eyelids open. Cold water may be used. Get medical attention immediately. Finish by rinsing thoroughly with running water to avoid a possible infection. Skin Contact: In case of contact, immediately flush skin with plenty of water for at least 15 minutes while removing contaminated clothing and shoes. Cover the irritated skin with an emollient. Cold water may be used. Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical attention immediately. Serious Skin Contact: Wash with a disinfectant soap and cover the contaminated skin with an antibacterial cream. Seek immediate medical attention. Inhalation: If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical attention immediately. Serious Inhalation: Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-to-mouth resuscitation. WARNING: It may be hazardous to the person providing aid to give mouth-to-mouth resuscitation when the inhaled material is toxic, infectious or corrosive. Seek medical attention. Ingestion: If swallowed, do not induce vomiting unless directed to do so by medical personnel. Never give anything by mouth to an unconscious person. Loosen tight clothing such as a collar, tie, belt or waistband. Get medical attention immediately.

Section 5: Fire and Explosion Data Flammability of the Product: Non-flammable. Products of Combustion: Hazardous decomposition include Nitric oxide, and ammonia fumes Explosion Hazards in Presence of Various Substances: Non-explosive in presence of open flames and sparks, of shocks. Special Remarks on Explosion Hazards: Forms explosive compounds with many heavy metals such as silver, lead, zinc and their halide salts. It can form shock sensitive compounds with halogens, mercury oxide, and siliver oxide.

Section 6: Accidental Release Measures Small Spill: Dilute with water and mop up, or absorb with an inert dry material and place in an appropriate waste disposal container. If necessary: Neutralize the residue with a dilute solution of acetic acid. Large Spill: Corrosive liquid. Poisonous liquid. Stop leak if without risk. Absorb with DRY earth, sand or other non-combustible material. Do not get water inside container. Do not touch spilled material. Use water spray curtain to divert vapor drift. Use water spray to reduce vapors. Prevent entry into sewers, basements or confined areas; dike if needed. Call for assistance on disposal. Neutralize the residue with a dilute solution of acetic acid. Be careful that the product is not present at a concentration level above TLV. Check TLV on the MSDS and with local authorities.

Section 7: Handling and Storage Precautions: Keep locked up.. Keep container dry. Do not ingest. Do not breathe gas/fumes/ vapor/spray. Never add water to this product. In case of insufficient ventilation, wear suitable respiratory equipment. If ingested, seek medical advice immediately and show the container or the label. Avoid contact with skin and eyes. Keep away from incompatibles such as metals, acids.

Storage: Keep container tightly closed. Keep container in a cool, well-ventilated area. Do not store above 25C (77F).

Section 8: Exposure Controls/Personal Protection Engineering Controls: Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location. Personal Protection: Face shield. Full suit. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves. Boots. Personal Protection in Case of a Large Spill: Splash goggles. Full suit. Vapor respirator. Boots. Gloves. A self contained breathing apparatus should be used to avoid inhalation of the product. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this product.

Section 9: Physical and Chemical Properties Physical state and appearance: Liquid. Odor: Ammonia-like (Strong.) Taste: Acrid. Molecular Weight: 35.05 Color: Colorless. pH (1% soln/water): 11.6 [Basic.] This is the actual pH in a 1 N solution. Melting Point: -69.2C (-92.6F) Specific Gravity: 0.898 (Water = 1) Vapor Pressure: 287.9 kPa (@ 20C) Odor Threshold: 5 - 50 ppm as ammonia Dispersion Properties: See solubility in water Solubility: Easily soluble in cold water.

Section 10: Stability and Reactivity Data Stability: The product is stable. Conditions of Instability: Incompatible materials, high temperatures Incompatibility with various substances: Highly reactive with metals. Reactive with acids. Slightly reactive to reactive with oxidizing agents. Corrosivity: Extremely corrosive in presence of zinc, of copper. Corrosive in presence of aluminum. Non-corrosive in presence of glass, of stainless steel(304), of stainless steel(316). Special Remarks on Reactivity: Incompatible with the following: Organic acids, amides, organic anhydrides, isocyanates, vinyl acetate, epichlorhydrin, aldehydes, Acrolein, Acrylic acid, chlorosulfonic acid, dimethyl sulfate, fluorine, gold + aqua regia, hydrochloric acid, hydrofluoric acid, hydrogen peroxide, iodine, nitric acid, olelum, propiolactone, propylene oxide, silver nitrate, silver oxide, silver oxide + ethyl alcohol, nitromethane, silver permanganate, sulfuric acid, halogens. Forms explosive compounds with many heavy metals (silver, lead, zinc) and halide salts. Special Remarks on Corrosivity: Dissolves copper and zinc. Corrosive to aluminum and its alloys. Corrosive to galvanized surfaces. Severe corrosive effect on brass and bronze Polymerization: Will not occur.

Section 11: Toxicological Information Routes of Entry: Absorbed through skin. Dermal contact. Eye contact. Inhalation. Ingestion. Chronic Effects on Humans: MUTAGENIC EFFECTS: Mutagenic for bacteria and/or yeast. [Ammonium hydroxide]. May cause damage to the following organs: mucous membranes, skin, eyes. Other Toxic Effects on Humans: Very hazardous in case of skin contact (corrosive, irritant, permeator), of ingestion, . Hazardous in case of eye contact (corrosive), of inhalation (lung corrosive).

Special Remarks on Chronic Effects on Humans: May affect genetic material based on tests with microorganisms and animals. May cause cancer (tumorigenic) based on animal data. No human data found at this time. (Ammonia, anhydrous) Special Remarks on other Toxic Effects on Humans: Acute Potential Health Effects: Skin: Causes severe irritation. Causes skin burns. May cause deep, penetrating ulcers of the skin. Contact with skin may cause staining, inflammation, and thickening of the skin. Eye: Contact with liquid or vapor causes severe burns and possible irreversible eye damage including corneal injury and cataracts. Inhalation: Causes severe irritation of the upper respiratory tract with coughing, burns, breathing difficulty. May cause acute pulmonary edema, pneumoconiosis, fibrosis, and even coma. It is a respiratory stimulant when inhaled at lower concentrations. It may also affect behavior/ central nervous system (convulsions, seizures, ataxia, tremor), cardiovascular system (increase in blood pressure and pulse rate). Ingestion: Harmful if swallowed. Affects the Gastrointestinal tract (burns, swelling of the lips, mouth, and larynx, throat constriction, nausea, vomiting, convulsions, shock, and may cause severe and permanent damage), liver, and urinary system (kidneys) May affect behavior (convulsions, seizures, ataxia, excitement). Chronic Potential Health Effects: Ingestion: May cause effects similar to those of acute ingestion. Inhalation: Repeated exposure to low concentrations may cause bronchitis with cough, phlegm, and/or shortness of breath. May also cause liver and kidney damage, and affect the brain, and blood. Eye: May cause corneal damage and the development of cataracts and glaucoma. Skin: Repeated skin contact to low concentrations may cause dryness, itching, and redness (dermatitis) Protective Equipment: Gloves. Full suit. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Wear appropriate respirator when ventilation is inadequate. Face shield.

V.

TOOLS and MATERIALS A. Tools :

Volumetric pipette 25mL

Volumetric flask 250mL Beaker glass 100mL Pipette

B. Materials: VI. NH3 solution Aquades

FLOWCHART

25 % NH3 - Take 37,6789 mL by using volumetric pipette in acid room - Poured into volumetric flask 100 mL 37,6789 mL NH3 25 % - Added aquades until reach half apart of volumetric flask - While shake it slowly, in order to make it be homogenous mixture (perfectly mixed) NH4OH solution - Added aquades again until reach sign line in measure flask

250 mL NH4OH 25% diluted VII. PROCEDURE 1. Calculating the mass of NH3 which is required to prepare 250 mL of NH4OH 2 M . Then it is obtained 903 gram for NH3 2. Converting mass of NH3 obtained into concentration. And the concentration obtained is 13,279 M 3. Calculating the volume of NH3 from the concentration, 13,279 M. Then, finding the volume of NH3 is 37,6789 mL 4. Pouring NH3 into volumetric flask 37,6789 mL by using volumetric pipette 5. Diluting NH3 by adding aquades half portion of volumetric flask 6. While shaking until the solution be homogenous mixture (perfectly mixed)

7. Adding aquades again into volumetric flask until reach the sign line.

VIII. RESULT AND DISCUSSION

NH4OH solution is the solution that prepared from NH3 in liquid phase. Where the preparation of solution is diluting solution by adding aquades. In this experiment, the volume needed of NH4OH 2 M is 250 mL. Before preparing the solution of NH4OH . the calculating of concentration and volume must be done. To calculate the concentration, volume of NH3 that required by using this formulation. Known % NH3 = 25% NH3 = 0.903 kg/L Asked V NH3 needed to make NH4OH solution 2M 250 mL? Answer 1. Determine the molarity of source solution. 2. Determine the V of source solution needed to make NH4OH solution 2M 250 mL Determining the molarity of source solution. Mass NH3 in 1L (g) = V (mL) x (g/mL) = 1000 x 0.903 = 903 g Mass NH3 in NH3 25% (g) = percentage (%) x mass (g)

Molarity (M)

25 x 903 = 225,75 g 100

mole Volume( L)

mass xV Mm 225.75 x1 17
= 13.279 M Determining the Volume of source solution needed
M 1.V1 M 2V2

V1

M 2V2 M1

V1

2 x 250 13.279

V1 37.6789mL

37,6789 mLof NH3 is poured into volumetric flask by using volumetric pipette. And diluted it by adding aquades for half portion initially of volumetric flask. And shaking for while time , in order to make the solution be homogenous mixture. After the solution perfectly mixed, adding aquades into that mixture until reach the sign line (250 mL). Finally, 250 mL of 25 % NH4OH 2 M solution have already prepared. And the color of solution is colorless. And then labeling the solution on the volumetric flask. IX. CONCLUSION : Preparation 250 mL of 25% NH4OH 2M is needed NH3 37,6789 mL. And it is also accompanied with diluting process.

ATTACHMENT PICTURE

Figure 1. Taking solution of NH3 in acid room

Figure 2. poured solution in volumetric flask

Figure 3. adding aquades just half portion of volumetric flask (diluting process)

Figure 4. NH4OH solution have been prepared by adding aquadest again until reach the sign line

REFFERNCES Grow HOW. 2008. Material Safety Data Sheet Amonia Solution. (Online) http://www.growhow.co.uk/documents/chemicalproducts_psds/ammonia_solution_msd s13aug08.pdf. Accessed on 05 March 2014 at 10.23 WIB Mitarlis, Utiya Azizah, dan Amaria. 2010. Organisasi dan Manajemen Laboratorium Pendidikan Kimia. Surabaya: UNESA University Prees. Puspita, Fika. 2013. Laporan Pembuatan Larutan. (Online) http://fikapuspita.blogspot.com/2013/07/laporan-pembuatan-larutan_9195.html. Accessed on 06 March 2014 at 11.47 WIB