Chemical Laboratory’s

Safety Instruction – Equipment – Test procedure

Prepared by :-
Mr. Bhavesh R. Rana
Jr. Officer Technology Group
Outline of Presentation
- Safety direction

- General lab equipment's

- Test procedure ( For 13” Mill )

 PH of Emulsion
 Conductivity of Emulsion
 Oil amount from Emulsion
 Determination of Fe contain from Emulsion
 Determination of Acid number of Emulsion
 Determination of SAP value of Emulsion
 Determination of chloride contain of Emulsion
 Safety Related Instruction
 Why accidents happen ?
Careless Inadequate Inadequate
Safety Training Instructions

Unsafe Over crowding

Experiments

Inadequate Facilities
Inadequate Equipment

Inadequate
Misbehavior Preparation
Ignorance

Poor Laboratory Teaching

Management Experiences
Do not
 Use damaged glassware
 Store chemicals near heat, sunlight, or other substances with
which they might react
 Store materials on floors or other places where people could
trip over them
 Leave equipment unattended when its operating (unless it is
designed to do so or you have an SOP)
 Put custodians and fellow workers in danger
 Use correct protective clothing and equipment

 Eye Protection
 Safety glasses – flying particles, chemical splashes, dust
 Splash goggles – corrosive liquids, solvents, powders
 Face Shields – high pressure systems

 Skin and Body Protection

 Gloves
 Aprons and lab coats – strong acids and bases
 Shoes – always worn in lab, closed toe and closed heel
 If Overexposed to a Hazardous Substance

Get medical help immediately!

Inform your lab supervisor
Check first-aid instructions.
Some general guidelines are
 Eyes: Flush with water for 15 minutes
 Ingestion: Follow label and MSDS instructions
 Skin Contact: Stand under emergency shower and remove
contaminated clothing immediately
 Inhalation: Get to fresh air and get prompt medical attention
 Materials
 Obtain the minimum amounts needed for your
work
 Ensure that all containers are clearly labelled
with their contents and a hazard label
 Toxic materials must be locked away
 Corrosive substances must be stored securely at a
low level in bunded trays
 Keep flammable materials in specially designed
cupboards and only have out the minimum for
immediate use (<50L per room)
 Store acids, bases & solvents separately
  Chemical Labels
 Every container of chemicals is labeled by the
manufacturer.

 The label will tell you

 Name of chemical
 Name, address and emergency phone
number of manufacturer
 Physical and health hazards
 Precautionary measures
 First-aid instructions
 Proper handling/storage instructions
 Typical Precautionary Measures on a Label
 Do not breathe vapors

 Use in well-ventilated areas

 Keep container closed when not in use

 Avoid contact with skin

 Wash thoroughly with soap and water after handling

 Keep away from sparks, heat, and flame

 Do not store near combustible materials

 Store in tightly closed container

 Remove and wash contaminated clothing promptly

 Keep from contact with clothing and other combustible materials

 Common Signal Words on Labels
 Danger – Can cause immediate serious injury or death
 Warning – Can cause potentially serious injury or death
 Caution – Can cause potentially moderate injury
 Color and Number Coded Label
Systems Colors represent kind of hazard
NFPA-type label • Red = fire
• Yellow = instability
• Blue = health
3 • black = specific hazard
& personal protection
4 2
Numbers show degree of hazard
• 0 = Minimal
• 1 = Slight
• 2 = Moderate
• 3 = Serious
• 4 = Severe
 Color and Number Coded Label Systems
NFPA-type labels
Black = specific hazard
• OX = Oxidizer

3 • ACID = Acid
• ALK = Alkali
4 2 • COR = Corrosive
COR • W = Use no water
• Other symbols:
 When in doubt – ASK!!!
Do not carry out a new
or unfamiliar procedure
until you have been
fully trained &
understand the
precautions necessary
for safe working
DO NOT GUESS!!!!
 Lab Equipment's
Beaker

 a flat-bottomed cylindrical
container, usually with a pouring
lip, to measure, mix, and prepare
liquids.
Flask

 a bottle, usually of glass, having a

rounded body and a narrow neck,
used especially in laboratory
experimentation.
Graduated Cylinder

 a narrow, cylindrical container

marked with horizontal lines to
represent units of measurement and
used to precisely measure the
volume of liquids.
Pipette or Dropper

 a slender graduated tube used in a

laboratory for measuring and
transferring quantities of liquids
from one container to another.
Goggles
 large spectacles equipped with
special lenses, protective rims, etc.,
to prevent injury to the eyes from
flying objects, bubbling liquid, or
any other potential threat in the lab.
Glass Stirring Rod

 A glass, cylindrical-like stick that

is used to mix solutions in a
beaker. Also referred to as a
“Swizzle Stick”
 Florence Flask
 Used to boil liquids.

 Also used to collect gases, if

applicable.

 Sizes vary.
 Volumetric Flask
 Used to prepare precise standard
solutions.

 They are only good for 1 specific

volume.

 Comes in many sizes

 Reagent Bottle
 Used to store, transport, or view
reagents such as acids or bases.
 Test Tube Brushes
 Cleaning.

 You must clean tubes before

and after you use.
 Thermometer
 Measuring temperature.
 Conductivity Meter
 Measuring conductivity.
 PH Meter
 Measuring Acidic and basicity
value.

 PH
 Hot Plate
 Used to heat substances.
 Watch Glass
 Used to show chemical reactions.
 Funnel
 Used to safely transfer substances
from one container to another.
 Wash Bottle
 Usually contains deionized water.

 Handy for rinsing glassware and for

dispensing small amounts of dH2O
for chemical reactions.
 Digital Balance
 Used to accurately measure mass.

 Only up to 200g in our labs.

Test Tube
 a hollow cylinder of thin glass with
one end closed, used for
experiments in labs.
Bunsen Burner
 a type of gas burner, commonly
used in chemical laboratories, with
which a very hot, practically
nonluminous flame is obtained by
allowing air to enter at the base and
mix with the gas.
 Determination procedures for
various properties of Emulsion
(Coolant)
 PH
PURPOSE : This method is applicable for the determination of pH values in
the range of 1-13 of aqueous systems, which do not contain materials
harmful to glass, such as fluorides.

APPARATUS : i. pH meter – Preferably digital, accurate to 0.01 or better.

ii. pH Electrode – Combined glass electrode or equivalent.
iii. Glass Beaker - 150ml.
iv. Thermometer – Calibrated thermometer ranging from 0 to
100 deg. c having subdivisions of 1deg.

CHEMICALS : i. Water - Distilled or De-mineralized.

ii. Buffer Solutions – Buffer Solutions having pH values of 4, 7
and 9 are needed for calibration of the pH meter.
 PH
i) Set the pH meter to the stand by mode.
ii) Thoroughly clean the electrode tip with water and wipe to almost dry.
iii) Immerse the electrode in a buffer Solution, having a pH of 7 and
adjust the scale reading to 7.00, according to the manufactures
instructions.
iv) Rinse the electrode tip with water and wipe to almost dry.
v) Immerse the electrode in a buffer Solution having a pH of 4 or 9
(depending on expected pH of the sample to be tested), and adjust the
scale reading, according to the manufactures instructions.
vi) Rinse the electrode tip with water and wipe to almost dry.
vii) Immerse the electrode in the sample Solution to be tested, allow the
scale reading stabilize, and read the pH, accurate to 0.01.
viii) Thoroughly clean the electrode with distilled water and store it in
potassium chloride Solution 3 mol /l.
 Conductivity
PURPOSE : This method is applicable for the determination of conductivity
values in aqueous systems, which do not contain materials harmful to glass,
such as fluorides.

APPARATUS : i. Conductivity meter – accurate to 1 us/cm or better.

ii. Conductivity electrode
iii. Glass Beaker - 150ml.
iv. Stirrer - Magnetic or glass rod.
v. Water bath - capable of maintaining a temperature of 20
deg. c, independent of the ambient temperature.

CHEMICALS : a. Water - Distilled or De-mineralized. b. Potassium Chloride

Solution (0.01M) – dissolve 724mg water and dilute to 1 litre.
  Conductivity
i. Place a glass beaker of 150ml containing 0.01M potassium chloride (KCI)
Solution and a glass beaker containing the sample under test, in a water
bath, maintaining at 20 c.
ii. Pre-rinse the electrode with some KCI Solution 0.01M, using another glass
beaker.
iii. Immerse the electrode in the KCI 0.01M Solution, maintained at 20 c.
iv. Adjust the scale reading to 1278 us/cm. According to the manufactures
instructions.
v. Rinse the electrode with water several times.
vi. Rinse the electrode with a portion of the sample under test, several times.
vii. Immerse the electrode in the sample under test, maintained at 20 c.
viii. Allow the scale reading to stabilize and read the conductivity, accurate
to 1 s/cm.
ix. Thoroughly clean the electrode with distilled water.
 Oil Determination from Coolant

PURPOSE : This method describes the determination of the total oil

concentration in fresh and used rolling Solutions.

APPARATUS : a. Graduated Cylinder – 100 ml. b. Babcock bottle - 110 ml

c. Oven - Capable of maintaining a temperature of 90 C.
The internal height should be enough to accept Babcock
bottles.
CHEMICALS : Water, Nitric Acid/HCL
i. Measure 100 ml of homogenized Solution into a 100 ml graduated cylinder.
ii. Transfer 50 ml of this Solution into a Babcock bottle.
iii. Add 20 ml Nitric acid, under continuous agitation, to Babcock bottle.
iv. Add the remaining 50 ml of the Solution
v. Place the Babcock bottle in water bath, maintained at 90 deg C until a
distinct oil layer has been formed, over a clear or translucent aqueous
layer.
vi. If necessary, add some water to the Babcock bottle until the liquid level
reaches the 100ml mark.
vii. Keep the Babcock bottle sometime in the water bath at 90 deg. C until a
distinct layer is formed.

Note :-
i. Sample for testing must be collected from mill stand before roll bite.
Temperature of solution must be noted down.
ii. Report the amount of oil, accurate to 0.1 ml, and report this as the oil
concentration in percent by volume.
iii. The contamination in the acid split layer is expressed in ml dirt.
 Fe Determination from Coolant

PURPOSE : This method determinations the total iron content in an

Solution, regardless whether it originates from dissolved FE 2+ , FE 3+ , Iron
soaps, or metallic iron

APPARATUS : i. Graduated Cylinder – 10 to 25 ml.

ii. pH meter – Preferably digital, accurate to 0.01.
iii. pH Electrode – Combined glass electrode or equivalent.
iv. Glass Beaker
v. Burette – 50ml, divided in 0.1ml subdivision or equivalent.
CHEMICALS : i. Hydrochloric Acid - concentrated (AR)
ii. Nitric Acid (30-35%) – Dilute 500ml of concentrated nitric
acid to 1 litre of de-mineralized or distilled water.
iii. Buffer Hydroxide Solutions 40% – Dissolve 400 gm
of Sodium hydroxide (AR) in 6000ml of distilled or
de-mineralized water.
 Fe Determination from Coolant
i. Add 50ml solution into a 250ml beaker.
ii. Add 15ml of concentrated HCI, put to hotplate and boil the mixture till the oil
colour has changed from grey to brown. This ensures that all iron soaps are
decomposed.
iii. Filter the mixture to remove the separated oil.
iv. Place a magnetic rod in the Solution and the beaker on a magnetic stirrer
with pH electrodes into the Solution.
v. Add 1 ml of the 5% sulfosalicylic acid Solution. If iron is present the colour will
change from yellow to red.
vi. While mixing add drop wise 40% sodium hydroxide Solution until a pH of 2 to
2.5 is reached. Should accidentally the pH become more than 2, correction can
be made using 35% Nitric acid.
vii. Allow the Solution to cool to room temperature.
viii. Titrate the Solution with 0.1m EDTA until the colour changes into yellow.
ix. Read the amount of EDTA necessary to obtain the colour change.
Calculation the iron content of the Solution as follows : -
(A X B X 55.8 X 1000)/C mg/ltr.
Where
A=ml EDTA Solution used for titration. C=ML used for iron determination.
B=Normality of EDTA Solution. 55.8 = Molar weight of iron.
 Determination SAP value of
Coolant
PURPOSE : This method describes the determination of the saponification
number for products, which are sufficiently light coloured to be titrated with
the use of an indicator.

APPARATUS : i) Balance ii) Titration Flasks iii) Glass beads. iv) Volumetric
pipette – 25ml accurate to 0.025ml or better. v) Condensers –
Liebig condenser of sufficient length. vi) Heating equipment –
continuous variable hotplate (for Erlenmeyer flasks) or heating
mantle (for round flask.) vii) Burette vii) Magnetic stirrer
Optional.

CHEMICALS : a. Enthanolic Potassium hydroxide (0.5m) b. Hydrochloric acid

(0.5M) c. Hydrochloric acid (0.5M) d. Isopropyl - AR Grade. E.
Isopropyl - AR Grade.
 Determination SAP value of
Coolant
i) Weight 1-2 g of the sample accurately to 0.01 gram into two Erlenmeyer flask.
ii) If the enthanolic potassium hydroxide Solution is not clear, filter it through a
folded filter paper directly before use. Filter an adequate volume to run all
sample tests and blank test (s).
iii) Add up to 10 glass beads to each Erlenmeyer flask to avoid retardation of
boiling.
iv) By means of a volumetric pipette, add 25ml of ethanolic KOH Solution to
both the flask containing the oil. Also put 25 ml of enthanolic KOH to another
Erlenmeyer flask which is considered as blank. Flush the inside wall of the
Erlenmeyer flask with a few ml IPA to prevent formation of a KOH residue
on the wall.
v) Place a condenser on each Erlenmeyer flask and boil with reflux on a
hotplate for 30minuets (depending on the sample; the boiling time should be
specified.)Take the Erlenmeyer flask + condenser from the hotplate.
vi) While the condensers still being installed on the Erlenmeyer flask, immediately
rinse the condensers with 50ml neutralized isopropyl alcohol and let it cool to
room temperature.
vii) Remove the condenser and add 5-10 drops of indicator Solution (a) and one
drop Methylene blue. Also add a magnetic follower (if a magnetic
follower or a magnetic stirrer is available).
 Determination chloride contain
of Coolant
viii) Titrate with 0.5(N) hydrochloric acid under continuous gentle agitation
(by hand swirling or with a magnetic stirring. The colour changes from blue
to green indicates endpoint is reached.

Calculate the saponification number of the sample as follows:-

Sap no = (A-B) x C x 56.11 (mg KOH/gm)
D
Where,
A=ml HCL Solution used for blank titration.
B= ml HCL Solution used for sample titration.
C= Normally of HCL Solution.
D=Sample weight in grams &
56.11=mol. weight of KOH.
 Tramp oil determination from
Coolant
Percentage of Tramp oil:-
The % tramp oil = (Sap of fresh oil – Sap of extracted oil) X 100
Sap of fresh oil

The reason for determining the total oil concentration and

the SAP number of the oil in the SOLUTION is to obtain
the percentage of active rolling oil present and the
percentage of tramp oil present
 Acid No. Determination from
Coolant
PURPOSE : This method describes an acid number determination suitable for
samples that are completely soluble in isopropyl alcohol at room temperature.

APPARATUS : i. Burette – A 50ml, burette graduated in 0.1ml subdivisions or

equivalent.
ii. Conical Flash – 250ml.
iii. Graduated Cylinder – 50 or 100ml size.
iv. Balance – Top scale/single pan model, accurate to 0.01 gram
or better.
CHEMICALS : i. Isopropyl Alcohol (IPA) – AR Grade.
ii. Potassium hydroxide Solution –0.1 (N) standardized
iii. Indicator Solution – Dissolve 0.1 gram Phenolphthalein in 100ml
ethanol 96%.
 Acid No. Determination from
Coolant
i. Weight 1-2 grams of the sample, accurately measured to 0.01 gram, into a
250ml conical flask.
ii. Add 40ml IPA and stir until the sample is completely dissolved .If necessary,
heating can be applied to facilitate sample dissolution, provided that the
sample material is not affected.
iii. The Solution must be cooled to room temperature prior to titration. If metals
separate out on cooling a more suitable test method must be chosen.
iv. Add 5-10 drops of indicator Solution.
v. Titrate immediately with 0.1(N) potassium hydroxide Solution. Apply gentle
mixing to avoid dissolution of carbon dioxide from air into the solvent. The color
changes from colourless to pink as the endpoint is reached.
vi. Consider the endpoint definite if the colour changes persists for 15 second.

Calculate the Acid Number of the sample as follows:-

Acid number = (A X C X 56.11) / D (mg KOH/g)

A=ml KOH Solution used for sample titration.
C= Normally of KOH Solution.
D=Sample weight in grams.
56.11=Molecular weight of KOH.
 Chloride Determination from
Coolant
PURPOSE : This method has been developed to determine chloride content in
the rolling oil Solution. It involves the chloride ions, present in the coolant,
being treated with an excess of silver nitrate and the residual silver nitrate
being determined by titration with ammoniumthiocyanate Solution. The
chloride content is then calculated.

APPARATUS : i. Graduated Cylinder – 10 to 50 ml.

ii. Hotplate
iii. Glass beaker – 150ml
iv. Burette – 50ml, divided in 0.1ml subdivisions or
equivalent.
CHEMICALS : i. Hydrochloric Acid HCI ii. Conc. Nitric acid (HNO3)
iii. Nitrobenzene solvent iv. Silver nitrate, standard
Solution (0.0564M) v. Ammoniumthiocyanate
standard Solution (0.0564N) vi. Ferric alum indicator
Solution – Dissolve 40gm of ferric
ammoniumsulphate.
 Chloride Determination from
Coolant
i. Add 50ml solution into a 250ml beaker.
ii. Add 15ml of concentrated HNO3 put to hotplate and boil the mixture till
the oil colour has changed from grey to brown.
iii. Filter the mixture to remove the separated oil.
iv. Add 25 ml silver nitrate to the filtrate and shake well.
v. Add 1 ml of Triethanolamine or nitrobenzene (Note 4) and 1 ml of ferric
alum indicator. Shake vigorously to coagulate the precipitate.
vi. Back titrate the excess silver nitrate present with freshly standardized
0.0564N.
Ammoniumthiocyanate, by means of a burette,
to a salmon pink point.

Calculate the chloride content as shown.

Mg/L CI = (25 * 0.0564N AgNO3) – (Burette reading * 0.0564N NH4CNS) X 40
0.0564 0.0564
 Any Questions ?