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Laboratory Practices Manual

1. SAFETY

It is the responsibility of the laboratory safety officer or his alternate to acquaint visitors and new employees with the safety features and policies of the lab. Each employee or visitor is then responsible for conducting himself in a safe manner according to the policies described below or as may be defined from time to time by the lab safety officer.

The laboratory includes the following safety features:

 

1. EMERGENCY SHOWER

A person who has been badly splashed with corrosive liquid should be quickly doused under the shower. They may be in a state of shock, or be unable to locate the shower themselves - so direct intervention may be needed. Their clothes should be removed quickly without regard to modesty. A clean pair of coveralls is available in the lab, but may only be used after thorough rinsing of the affected area.

2. EYE WASH STATION

The eye-wash station should be used for all splashes into the face and eyes. Thorough flushing of the eyes is essential for even minor splashes.

3. FIRE EXTINGUISHER (Dry Chemical)

A dry chemical (class ABC) fire extinguisher is appropriate for all types of minor fires. Pull the pin on the side of the handgrip, direct the nozzle at the base of the flame and squeeze the handgrip. Stand at a safe distance.

4. EMERGENCY EXITS AND TELEPHONE

Two exits are provided. A telephone is provided in the office, and a list of emergency numbers is mounted on the wall above the phone.

5. MSDS SHEETS

Material safety data sheets are available on all raw materials and products. They are found in a series of red binders in the lab. Reference books are also available, such as "Dangerous Properties of Industrial Materials, 5th Ed." by Sax.

6. FUSE BOX

In case of electrocution or electrical fire, the appropriate circuit may be turned off from the fuse box. DO NOT TOUCH A VICTIM OF ELECTROCUTION BEFORE SHUTTING OFF THE POWER.

7. SAFETY POLICIES

All dangerous experiments as well as experiments which may spread an obnoxious odour should by done in the fume hood.

Smoking, eating and drinking are forbidden in the laboratory.

Safety glasses should be worn at all times. Users of contact lenses should be aware that vapours will absorbed by the lens and may lead to severe irritation and damage to the cornea if not dealt with promptly. Contact lenses should therefore not be worn in the laboratory.

Laboratory coats are strongly recommended.

Disposable gloves are available and should be used.

Broken glass must be disposd of in the bin provided - not in the general waste bin.

Any injury, no matter how slight, should be recorded in the Worker’s Compensation Board "Incident Report Book". A First-Aid kit is available if needed.

Good housekeeping should be practised at all times. Benches should be kept uncluttered and isles unplugged.

Spills should be cleaned up as soon as possible. A spill kit is available.

Flammable liquids should be stored in the cupboard provided.

Acids and bases should be stored separately and in the cupboards provided.

Compressed gas cylinders should be kept secured in their rack.

Solid wastes must be collected in the container provided and should never be dumped into the garbage.

Aqueous wastes should be flushed down the sink with plenty of cold water.

Organic liquid wastes should be separated into chlorinated and non-chlorinated. A container is provided for each. They should never be poured down the sink.

2. ORGANIZATION / PERSONNEL

The laboratory is responsible for the following:

• analytical quality control
• process control
• process development
• waste treatment
• soil and tissue testing
• other spects of contract formulating and quality control.

There is one chemist on staff Mr. Paul Warren.

3. FACILITIES

The laboratory complex inclus 480 square feet of lab space, 130 square feet of storage, and 160 square feet of office space.

The lab is well equipped with utilities, will lit, temperature controlled and well ventilated by positive pressure. No reagent grade water is available "on tap" because of insufficient demand. Bottled water is used.

Storage is provided for samples awaiting analysis, and for retained samples. Analytical standards are kept in a desiccator or in the refrigerator as required.

4. EQUIPMENT

See attached list

5. MAINTENANCE AND CALIBRATION
1. Analytical Standards

All analytical standards must be stored in the refrigerator or inside a dessicator. To reduce handling to a minimum, a working vial of each standard should be used. Both these should be labelled with date, and whether it is a main vial or a working standard.

2. Reagents

Written procedures exist for reagent preparation in this manual. All reagents must be labelled with identity, date of preparation, and the analyst concerned.

3. Maintenance Manuals

Maintenance for lab equipment is conducted using a PC based maintenance program. All information on routine and demand maintenance is kept indefinately.

4. Calibration / Maintenance Procedures

HPLC: The HPLC's are calibrated for each assay. Maintenance is on an "as needed" basis. We have no contract. At least once a year a known sample of each analyte must be run and shown to be within statistical limits using a Shewart Chart or other statistically valid means.

GLC: The GLC is calibrated for each assay. Maintenance is on an "as needed" basis. We have no contract. At least once a year a known sample of each analyte must be run and shown to be within statistical limits using a Shewart Chart or other statistically valid means.

ANALYTICAL BALANCE:The analytical balance should be calibrated every two years by a qualified technician. The built-in calibration should be used at least once a week. Maintenance is on an "as needed" basis.

SPECIFIC GRAVITY BALANCE: The specific gravity balance should be calibrated with distilled water at 20.0 degrees Celsius every week.

CORNING pH METER: The pH meter should be calibrated at two points every time it is used. Maintenance is on an "as needed" basis.

FISHER CONDUCTIVITY METER: This unit should be calibrated, as outlined in the procedure 93-04-INH, before each batch of samples is run.

6. METHODS / PROCEDURES

All methods and procedures used in the lab must be written up and included in the library of methods. All methods and procedures must be validated by at least one of the methods given in the statistics section of the lab manual. Old methods and specifications must be retained in the appropriate master file.

Analytical methods are divided into the following volumes:

• The master book of Sidekick (Monsanto) quality control and specifications.
• Sidekick Analytical Methods ( R )
• Sidekick Analytical Methods (AI)
• Sidekick Analytical Methods (OR)
• ORTHO Formulation Test Methods.
• A Laboratory Manual for the Chemical Analysis of Waters, Wastewaters, Sediments and Biological Materials (2nd Edition), B.C. Ministry of the Environment.
• Official Methods of Analysis, 14th Edition, AOAC 1984 (plus updates).
• U.S. EPA Manual of Chemical Methods for Pesticides and Devices.
• U.S. EPA Test Methods for Evaluating Solid Waste (1980).
• Vogel’s Textbook of Quantitative Inorganic Analysis, 4th edition.
• Vogel’s Textbook of Macro and Semimicro Qualitative Inorganic Analysis, 5th edition.
• Later Chemicals laboratory methods for analysis of pesticides (1994).

Always follow the methods carefully.

7. RECORDS

A 250 mL sample of each batch is taken by the formulator immediately after the batch has been completed (ie. after adequate mixing has occurred). It is the formulators responsibility to properly label each sample with product, lot number, date, time, and then sign the tag. He then must deliver the lavelled sample to the lab.

All raw data and calculations should be recorded by the analyst in the appropriate lab notebook for future reference. No scraps of paper should be used. The analyst must record the date, product and batch concerned.

The final analytical report issued by the lab should include product, batch , date formulated, formulator, date analyzed, and analyst. The analytical methods used should be quoted. The analyst must sign the report. These records must be retained for at least five years.

8. CORRECTIONS OF BATCH CONCENTRATION
1. If the batch is too high in concentration



Where:


C_r = Required Concentration of Active Ingredient
C_m = Measured Concentration of Active Ingredient
m = Total Mass of the Batch
m_x = Mass of Inactive Ingredient to Be Added
P = Purity of Active Ingredient

 

2. If the batch is too low in concentration



Where:


C_r = Required Concentration of Active Ingredient
C_m = Measured Concentration of Active Ingredient
m = Total Mass of the Batch
m_x = Mass of Inactive Ingredient to Be Added
P = Purity of Active Ingredient

9. QUALITY OF INCOMING MATERIALS

1. Certificates of analysis

If a certificate of analysis is provided for an active ingredient the C of A will be filed for five years in the lab and the batch will be formulated based on the C of A. If a C of A is not provided then the material will be sampled under the direction of a chemist and the concentration will be determined. The batch will then be formulated based on the determined concentration.

Later Chemicals purchasing Dept. will give preference first, to ISO certified suppliers, then suppliers who will provide C of A’s and who agree to be audited by Later’s technical staff and finally to suppliers who provide a C of A but will not agree to a QA/QC audit.

2. Quality of packaging

A sample of packaging materials of the size recommended by the Canadian weights and measures Dept. (based on the lot size) will be taken. These samples will be weighed to obtain a starting tare weight and to look for conformance to specifications.

In addition each sample will be inspected for colour and measured for conformance with specifications.

Customer requirements may differ and the lab is responsible for ensuring customer requirements are followed.

10. QUALITY OF FINISHED PRODUCT
1. Records

All products will have a product log book. In this book all records pertaining to the product run will be kept. The log will be stored for a minimum of five years.

2. SPC

Statistical methods will be used for weight controlon all products. Attribute charts for label placement and leaks will be used where required. If stability cannot be demonstrated an assignable cause must be found before packaging can continue.

3. Process capability

Process capability studies are highly recommended before packaging a new product. A capability index of 1.0 or greater is required.