Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Effective Date:
TITLE: Preparation of Solutions
APPROVING OFFICIALS:
DD / MM / YY
Approved By: _________________
Concurred By: _________________
Prepared By: _________________
Management
QAU Manager
___________
___/___/___
___/___/___
___/___/___
1.0 INTRODUCTION
1.1 Purpose
To assure reproducibility in preparation of solutions as well as adequacy
and consistency of documented calculations associated therewith.
1.2 Scope
This general-use technical SOP is a GLFC management directive that shall
be followed for all projects/studies of Natural Resources Canada, CFSGLFC, which prepare solutions in the conduct of GLP compliant studies.
1.3 Definitions
Archivist - The person specified by management who is responsible for the
management of the archive(s).
CFS-GLFC – Canadian Forest Service – Great Lakes Forestry Centre.
Document Control Official (DCO) - The person specified by management
who is responsible for controlling designated documents, including SOPs.
Effective Date - The date from which the procedures given in a SOP are to
be implemented.
Good Laboratory Practice (GLP) – A quality management system set forth
by the Organization for Economic Cooperation and Development (OECD) to
assure the quality and integrity of the processes and conditions under which
non-clinical health and environmental safety studies are planned,
performed, monitored, recorded, archived and reported.
Material Safety Data Sheet (MSDS) – a summary description of a
chemical, reagent or substance prepared by the manufacturer or supplier
which is required by WHMIS legislation to inform workers about procedures
required to safely work the material.
NA - Not Applicable.
Quality Assurance Unit (QAU) - Persons designated by management to
ascertain that the study is in compliance with current OECD Principles of
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Good Laboratory Practice, and who are completely independent from the
conduct of the study for which they are performing quality assurance
functions.
Reference item – Any item used to provide a basis for comparison with the
test item.
Standard Operating Procedures (SOPs) - Management directives
describing administrative or technical routine procedures conducted in a
laboratory or field operation that are not specified in detail in the study plan
or test guidelines.
Study Director – The individual responsible for the overall conduct of the
non-clinical health and environmental safety study.
Study Plan – A document that defines the objectives and experimental
design for the conduct of the study, and includes any amendments.
Test Facility Management – The individual who has the authority and
formal responsibility for the organization and functioning of the test facility
according to current OECD Principles of Good Laboratory Practice.
Test Material – An article which is the subject of a study, typically an
analytical grade, technical grade or formulated product which is uniquely
identified and characterized and which is tested in GLP compliant studies to
examine its properties, human and/or environmental safety.
Workplace Hazardous Materials Information System (WHMIS) – a
national information delivery system used to inform employees about
hazardous materials in the workplace.
1.4 Safety
1.4.1 Persons using solvents or other hazardous materials, must use
minimum personal protective equipment as stipulated in the current
version of SOP No. M52506/014, The Use of Personal Protective
Equipment.
1.4.2 Persons using any solvents, chemicals, reagents or other
hazardous materials must do so in accordance with the current
version of SOP No. M52506/015 The Safe Handling of Hazardous
Materials and pertinent MSDS sheets, which are stored on a shelf
in the laboratory and in accordance with WHMIS labels.
1.4.3 Decanting, transfer or other handling of large (>500 mL) containers
of solvents must be conducted in an approved operational fume
hood. Fume hoods should be approved or certified annually.
1.4.4 All persons must receive WHMIS training and be familiar with
emergency procedures as described in the CFS-GLFC Emergency
and Fire Safety Manual, prior to working in a laboratory using
hazardous materials. WHMIS and emergency procedure training as
well as records associated therewith are to be coordinated by the
CFS-GLFC Safety Officer.
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
1.5 Materials
The materials required to prepare solutions include:
1.5.1 GLP Form No. 0082/001 (Appendix 1) as well as GLP forms No.
0083/001, 0084/001, 0085/001 and 0086/001 (Appendices 2-5) with
sufficient open data rows for recording appropriate data and
calculations pertaining to the solutions being prepared.
1.5.2 At the discretion of the study leader or principal investigator, a
logbook for Preparation of Solutions and Serial Dilutions may be
prepared to compile and retain exact copies of all forms associated
with preparation off solutions. However, all original forms are
considered raw data and must be retained together with the study
records.
1.5.3 Selected solvent(s).
1.5.4 Appropriately sized glassware and hardware (e.g. volumetric flasks,
spatulas, pipettes, and weighing vessels), as required for
preparation of solutions involving either solid or liquid solutes.
1.5.5 All glassware used in preparation of solutions required for pesticide
residue analysis are to be cleaned in accordance with the current
version of SOP M52506/008.
1.5.6 Where micropipettes are to be employed, these must be certified,
maintained, calibrated and operated in accordance with the current
version of SOP M52506/018.
1.5.7 All glassware is to be pre-labeled in accordance with the current
version of SOP RS9701/001 and as mandated by WHMIS
legislative requirements.
1.5.8 Certified and calibrated top loading balance or analytical balance,
used and maintained in accordance with the current version of SOP
M52506/013 or M52506/017 respectively.
1.5.9 Vortex mixer, inert stirring instrument, magnetic stir bar and retrieval
rod and magnetic stir plate or hot plate maintained and used in
accordance with the current version of SOP M52506/022 as
required to ensure full dissolution of solutes and homogeneity of
solutions.
1.5.10 Indelible labels.
1.5.11 WHMIS labels.
2.0 PROCEDURES
2.1 General Procedures
2.1.1 Determine the type of solution and total volume required by
reference to the study plan or pertinent test method.
2.1.2 Follow required safety precautions for the specific solutes and
solvents being used by referring to the appropriate MSDS sheets,
and as set forth in the current version of SOP No. M52506/015, The
Safe Handling of Hazardous Materials and SOP No. M52506/014,
The Use of Personal Protective Equipment.
2.1.3 Prepare WHMIS compliant or indelible labels for each solution to be
prepared and affix to the container to be used for longer term or
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
temporary storage of the final solution respectively. Choice of the
type and size of the container to be used for final solutions will
depend upon the volume of solution required and its subsequent
use pattern. However, care should be taken to ensure that the
container material is inert to the solution components and that it is
clean. Choice of container type will depend upon the volatility of
the solute and solvent (influencing the type of closure required) and
subsequent use for the solution (e.g. requirement for immediate
use and decanting of measured portions may lead to use of a
graduated cylinder; whereas requirement for longer term storage
under refrigerated conditions may lead to use of a glass-stoppered
Erlenmeyer flask).
2.1.4 Use liquid measuring devices appropriate for the task (e.g.
graduated cylinder, graduated pipette, volumetric flask, volumetric
pipette etc.). Choice of appropriate devices will depend upon the
volume to be delivered and the overall accuracy and precision of
measured volumes required. As a general rule of thumb the total
volume of the measuring device should not be greater than ten
times that of the volume to be measured and delivered. Generally,
for preparation of routine solutions standard graduated devices may
be employed, whereas for solutions of reference and test materials
or those requiring high levels of accuracy should typically involve
the use of volumetric glassware and/or positive displacement
micropipettes.
2.1.5 Solvents and liquid solutes must be brought to ambient laboratory
temperature prior to volume measurement or use.
2.1.6 The exact amounts of the solutes and solvents required for each
solution must be calculated and recorded using version 001 of GLP
forms 0083 through 0086 (Appendices 2-5) depending upon the
method used to prepare the solution (refer to section 2.6).
2.1.7 All final solutions must be indelibly labeled with a minimum set of
information including: chemical name, concentration, solvent, date
prepared, initials of person preparing the solution and the expiry
date if applicable.
2.1.8 Do not return any unused solvent or chemical compound to the
original container. Store in an appropriate container, pre-labeled
according to WHMIS requirements, or discard it as set forth in the
current version of SOP No. M52506/006, Disposal of Hazardous
Waste.
2.1.9 Documenting and handling of original and exact copies of solution
preparation documents must be performed as described in section
2.6.
2.1.10 For solutions which constitute samples, test materials or reference
items, documentation of their creation or subsequent use must be
made in accordance with the current version of SOP M52506/025.
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Natural Resources Canada
CFS - GLFC
2.2 Preparation of
Measurements:
Solutions
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Involving
Solid
Solutes
and
Mass
2.2.1 Choose the appropriate type of balance for weighing out the solid
solute. Choice of balance type will depend upon the mass and
accuracy required for the specific solution. General-use solutions
may be prepared using a top loading balance. Solutions requiring a
higher degree of accuracy or which are being used as reference
items or test materials should be prepared using an analytical
balance unless logistically infeasible owing to large mass
requirements.
2.2.2 With appropriate compensation for the purity of the substance
being weighed, calculate the required mass of solute and volume of
solvent required to make the desired solution and record
calculations on GLP Form No. 0083/001.
2.2.3 Ensure the balance has been appropriately calibrated and use it to
tare a clean, appropriately-sized weighing vessel, such that a stable
zero reading is obtained.
2.2.4 Using a clean spatula or similar instrument, carefully transfer the
required amount of the solid solute into the weighing vessel,
ensuring that no spilled material is left on the balance pan or on the
outside of the vessel.
2.2.5 Quantitatively transfer the solute mass from the weighing vessel
into the final solution container. Add aliquots of solvent to rinse the
weighing vessel and transfer rinsates into the final solution
container to ensure quantitative transfer.
2.2.6 Add the majority of the required volume of the solvent to the final
solution container and mix the solution apparatus such that the
solute is fully dissolved and the solution is visibly homogeneous. In
cases where full dissolution of the solute may require heating or
extensive mixing, use of a temperature-controlled, magnetic,
hotplate/stirrer apparatus is recommended. Where no heating or
only minimal mixing is required dissolution and homogeneity may
be achieved by hand-swirling, vortex-mixing, stirring with an inert
instrument or by repetitive inversion.
2.2.7 Bring the solution to its required final volume by further addition of
the solvent and remix the complete solution to ensure complete
homogeneity. If a magnetic stir bar has been employed in mixing
remove it using a Teflon coated magnetic retrieval rod.
2.3 Preparation of
Measurement:
Solutions
from
Liquid
Solutes
Using
Mass
2.3.1 Ensuring that appropriate adjustment is made for purity, calculate
the required mass of the liquid solute required and record the
calculations on GLP Form No. 0083 /001.
2.3.2 Calibrate the balance chosen for this task and use it to tare a clean,
appropriately-sized weighing vessel, such that a stable zero
reading is obtained.
2.3.3 Using a clean, inert device (e.g. pipette, cylinder, beaker) transfer
the required amount of the liquid solute into an appropriate sized
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
weighing vessel, ensuring that no spilled material is left on the
balance pan or on the outside of the vessel.
2.3.4 Quantitatively transfer the weighed out solute into the final solution
container and use aliquots of the solvent to rinse the weighing
vessel with rinsates added into the final solution container.
2.3.5 Add the majority portion of the solvent to the final solution
container. In cases where full dissolution of the solute may require
heating or extensive mixing, use of a temperature-controlled,
magnetic, hotplate/stirrer apparatus is recommended. Where no
heating or only minimal mixing is required dissolution and
homogeneity may be achieved by hand-swirling, vortex-mixing,
stirring with an inert instrument or by repetitive inversion.
2.3.6 Bring the solution to final volume by further addition of the solvent
and remix the complete solution. If a magnetic stir bar has been
employed remove it using a Teflon coated magnetic retrieval rod.
2.4 Preparation of Solutions from Liquid Solutes by Volume Measurement:
2.4.1 Following the example provided in the top line of GLP Form No.
0084/001, and with reference to section 2.5 of this SOP, determine
and record the appropriate solvents and respective volumes
required for the solution being prepared.
2.4.2 Using a clean, inert, measuring device of appropriate volume and
accuracy, measure out the required volumes of each liquid
comprising the final solution.
2.4.3 Transfer the measured volume(s) of each of the liquid solutes into
the final solution container. In most cases involving liquid solutes
only minimal mixing is required to ensure complete dissolution and
homogeneity. This may generally be achieved by hand-swirling,
vortex-mixing, stirring with an inert instrument or by repetitive
inversion. Ensure the solution is visibly homogeneous prior to use.
2.5 Calculations
2.5.1 Significant Digits and Rounding
(a) All measurements/calculations will be taken to the number of
decimal places required as stipulated in the study plan.
(b) All numbers will be rounded.
(c) Rounding will be determined by the subsequent digit.
Example: If rounding to 2 decimal places:
If the number in the third decimal place is 5 or greater, the
number preceding it will increase by one, whereas if the number
in the third decimal place is less than 5, the number preceding it
will remain the same.
Example:
236.548 will be rounded up to 236.55 whereas 236.543
will be rounded to 236.54
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
2.5.2 Calculations for Preparation of a Solution Using a Weight:Volume
Approach
Follow the example on GLP Form No. 0083/001.
2.5.3 Calculations for Preparation of
Measurements and Ratio Notation
a
Solution
Using
Volume
Follow the example on GLP Form No. 0084/001.
Note that there are two common notation methods used in
preparing and documenting solutions, however they are often
mistakenly applied. For consistency and compliance with this SOP
ratio notation must be used, following the example line as shown on
GLP Form No. 0084/001. Using ratio notation a 1:10 solution of
ethanol and water (read and pronounced as a 1 to 10 solution of
ethanol and water). With this notation, the total number of parts of
the solution being the sum of the numbers (in this case is 1+10=11.
Thus 1:10 represents an 11 part solution of which 1 part is ethanol
(the solute) and 10 parts are water.
2.5.4 Calculations for Preparation of a
Measurements and Percent Notation
Solution
Using
Volume
Follow the example on GLP Form No. 0085/001.
2.5.5 Calculations for Preparation of Molar Solutions
Follow the example on GLP Form No. 0086/001.
2.6 Documentation and Reporting
2.6.1. Any solutions prepared must be recorded on GLP Form No.
0082/001 (Appendix 1). The original is to be maintained with the
study records and a copy may be maintained in the logbook for
Preparation of Solutions and Serial Dilutions. If the solution is a
test material or reference item, refer to section 2.6.3.
2.6.2. Calculations for preparation of any solution must be documented on
version 001 of the applicable form (i.e. one of GLP Forms
numbered 0083 through 0086 (Appendices 2-5) depending upon
methods used). The original of each form is to be maintained with
the study records. Exact copies may be compiled in a separate
logbook for solutions if desired.
2.6.3. In the case where the solution being prepared is a test material or
reference item, an exact copy of the record of solutions prepared
and associated forms for calculations for that solution must be filed
in the Test Materials and Reference Items Logbook.
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
3.0 DISTRIBUTION AND ARCHIVING
3.1 Distribution
3.1.1
3.1.2
3.1.3
Official copies of this SOP shall be made by the DCO and
distributed as follows:
(a) The original SOP and an exact copy shall be retained in the
GLFC archive (i.e., copies 001 and 002).
(b) One copy shall be kept by the DCO in the DCO SOP manual
(i.e., copy 003).
(c) One copy shall be kept by the QAU manager in the QAU
manager SOP manual (i.e., copy 004).
The DCO may distribute additional copies of this SOP to personnel
engaged in the supervision or conduct of GLP studies.
The DCO shall announce the availability of new versions of this
SOP within one week of the effective date, and shall distribute new
versions by requiring that old versions be exchanged for the new
ones.
3.2 Archiving
The Archivist shall maintain current and historical versions of this SOP.
3.3 Destruction of Outdated SOPs
With the exception of archived historical versions, the DCO shall ensure the
destruction of outdated versions of this SOP by shredding.
4.0 ASSURING SOP VALIDATION AND COMPLIANCE
4.1 SOP Validation
The QAU is responsible for assuring that this SOP is valid.
4.2 SOP Compliance
The Study Director is responsible for assuring that this SOP is followed.
5.0 REVISION OF THE SOP
5.1 Responsible Individual
The QAU is responsible for assuring that this SOP is current. If necessary,
the QAU manager shall initiate the revision process.
5.2 Revision Schedule
5.2.1
5.2.2
This SOP shall be revised when its provisions no longer agree with
current practices or applicable regulations.
If this SOP requires revision, it shall be revised according to current
GLFC procedures and approved within 45 calendar days of
initiation of the revision process.
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
6.0 CONTINGENCIES
When personnel find circumstances that do not permit compliance with this
SOP, they shall consult both the QAU manager and the Study Director.
7.0 CONFIDENTIALITY
All SOPs are considered confidential and shall be handled accordingly.
They are not to be copied or made available to outside parties without
proper safeguards and the approval of management. Distribution to outside
parties shall be conducted by the DCO.
8.0 REFERENCES
(a)
(b)
(c)
(d)
(e)
(f)
(g)
(h)
(i)
(j)
(k)
CFS-GLFC Emergency and Fire Manual
SOP No. M52506/014, The Use of Personal Protective Equipment
SOP No. M52506/015, The Safe Handling of Hazardous Materials
SOP No. M52506/013, Maintenance, Calibration and Operation of
Electronic Top Loading Balances.
SOP No. M52506/017, Maintenance, Calibration and Operation of
Analytical Balances.
SOP No. M52506/006, Disposal of Hazardous Waste.
SOP No. RS9701/001, General Laboratory Procedures
SOP No. M52506/008, Routine Cleaning of Laboratory Glassware and
Hardware
SOP No. M52506/018, Routine Operation, Calibration and Maintenance
of Micro-Pipettes
SOP No. M52506/022, Maintenance, Calibration and Operation of
Magnetic Stirrers/Hot Plates.
SOP No. M52506/025, Storage and Tracking of Samples, Test
Materials and Reference Items
9.0 APPENDICES
Appendix 1:
Appendix 2:
Appendix 3:
Appendix 4:
Appendix 5:
GLP Form No. 0082/001, Record of Solutions Prepared.
GLP Form No. 0083/001, Calculations for the Preparation of
Solutions Using Mass Measurements
GLP Form No. 0084/001, Calculations for the Preparation of
Solutions With Liquid Solutes Using Ratio Notation
GLP Form No. 0085/001, Calculations for the Preparation of
Solutions Using Volume Measurements and Percent
Notation
GLP Form No. 0086/001, Calculations for the Preparation of
Molar Solutions.
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Appendix 1
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CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Appendix 2
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CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Appendix 3
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CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Appendix 4
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Natural Resources Canada
CFS - GLFC
STANDARD OPERATING PROCEDURE
Preparation of Solutions
SOP Number: M52506/034/001
Appendix 5
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