Professional Documents
Culture Documents
Solutions - Solutions or Problems
Solutions - Solutions or Problems
30/Perfumer & Flavorist 0272-2666/00/0001-0030$06.00/0—© 2000 Allured Publishing Corp. Vol. 25, January/February 2000
SOLUTIONS: SOLUTIONS OR PROBLEMS?
rate than weighing 5 g at the perfumer’s bench because and the compounder to 1 kg on their 100 kg capacity
both have the same relative readability. More accurate balance. Older-style lever balances with analogue readouts
balances are available, but these are usually only suitable in can be more accommodating, because a fraction of a
low-traffic areas because of sensitivity to draughts and division can be seen, even if not accurately noted. How-
vibration, and are generally reserved for analytical depart- ever, without RS232 outputs, they have lost popularity in
ments rather than compounding areas. GMP procedures.
The second point of consideration is the degree of
General Principles
accuracy needed. How accurate does our weighing of
individual components in a compound really need to be? I In consideration of these factors, I recommend the follow-
polled several friends and colleagues in the business and ing guidelines to students when making samples or plan-
asked if they were aware of the tolerance their company ning for production batches of their formulations:
allowed when weighing individual materials during the
• There would seem to be a case for using solutions to
compounding of fragrances. All but one stated that they did
ensure accuracy when weighing amounts less than 1%
not know or were not aware of this having been quantified
of a formulation’s total. Of course using a range of
and I had no reason to believe they were being evasive on
balances for different weights does help to overcome
this issue. The one that stated the policy of his company told
this. If balances are cross-calibrated and the error
me, “There is no allowable tolerance…we weigh accurately
characteristics are determined, accuracy can be main-
every time.” These comments launched a series of experi-
tained. Using the mid range of a balance rather than
ments to determine how big an error is really necessary to
the limits of its capacity generally gives better results.
produce significant differences in the odor of samples.
Specifying which balances are to be used for specific
The experiments that followed showed that if accuracy
weight ranges also helps. The rule of two decimal
to the target weight can be maintained in the range of
places below (1% of target weight) is a good guide.
+/- 10%, then the resultant difference in the compound’s
odor, as evaluated by a panel of testers, was found to be • Equipment chosen for weighing should be able to
slight. In the case of more than one such error, particularly weigh to a readability of a decimal point that represents
if the materials had substantially different odor characters 1% of the target weight of that material. To weigh 0.1
from the finished compound, a detectable odor difference g, our balance ideally should have readability to 0.001
could occur. g. To weigh 37.23 g, the balance ideally should have
When the accuracy approached the range of +/- 1% of readability to at least 0.1 g. The small difference result-
the target weight, the resultant difference in the compound’s ing from not being able to weigh the last 0.03 g in these
odor was not detectable by the panel even in multiple guidelines my be regarded as a non-significant quan-
under- or over-doses within this range. This is easily cor- tity. Weighing 37.1 g on a 0.1 readability machine and
roborated by accurately weighing a compound and deliber- then 0.03 g on a 0.001 g readability machine is not a
ately making a second sample with the strongest or even guarantee that total accuracy will improve because the
most abundant material in the formula at +1% of target inherent inaccuracy in the larger machine may have
weight and a third sample at –1% of target weight. These already added an error greater than this in any case.
results were irrespective of the material’s abundance, • In view of the typical balance range found at the
strength, volatility or dilution. If the formula calls for 0.1% perfumer’s organ (200 g capacity with a 0.01 g readabil-
then the low figure is 0.099% and the high 0.101%. If the ity), the optimum minimum weighed in a 100 g sample
formula calls for 50% then the low is 49.5% and the high is 1 g. Therefore, this restricts formulas to use not less
50.5%. than 1% of any single material. However, for practical-
If we accept that 1% is an acceptable error (if we require ity with initial experimental samples, I suggest that this
even greater accuracy the argument becomes even more could be extended to 0.1% (0.1 g in 100 g), less than the
compelling), we should only weigh a material with weigh- ideal and certainly not accurate enough for trail or
ing equipment that is accurate to 1% of the target weight. sampling batches. If less than 1.0/0.1% is used, then
Given that the typical readability found on balances typi- that material is best used as a solution.
cally used in perfumery houses is 0.01% of capacity, using • Materials with an odor impact of 100 or less (where
the 1% rule means that the minimum quantity to weigh be linalool synthetic is the control with an odor impact of
limited to 100 x 0.01% or 1% of the capacity of the balance. 100) do not generally require dilution, unless they are
However, it is not as easy as using a smaller balance to less than 0.1% of the formula. Stocking dilutions can
weigh smaller-quantity items than this because the vari- take the odor impact down to about 100, the same
ance between different capacity balances may well intro- strength as linalool ( e.g. Cis-3-hexenol has an impact of
duce a second error that can be greater than the acceptable 700 [seven times the impact of linalool]). A 10% solution
1% target range in any case. This accuracy limitation is generally acceptable for most compounds. For con-
therefore would restrict the perfumer to weighing a vention and simplicity’s sake these are best kept as
minimum of 1 g on his or her two-decimal-place balance, multiples of 10.
• Solutions made only as 10% give that have passed QC ensures repro-
better uniformity of results, sub- ducibility.
ject to their solubility characteris- • Solutions in ethanol or other mate-
tics (some materials’ solubility may rials that are not inert and undergo
be too low to allow 10%, such as a maturation process or are dissolved
maltol, soluble at a maximum of in an odorous-materials process are
around 5% in DPG). While making best treated as distinctly separate
100 g of a 1% solution on a 200 g/ sub-compounds and standardized
0.01 readability balance, the 1.0 g in age and storage conditions before
indicated on the balance readout inclusion in their parent compounds.
could actually be in the range of
• A formula follows these guidelines
0.995 and 1.015, because the third
irrespective of batch size. If solu-
decimal place is unknown. Using
tion parameters fall out of these
the 10% rule, an extra decimal place
guidelines then they are best for-
of accuracy is added. A 1% solution
mulated as sub-compounds and
is made from 10% of a 10% solu-
labeled accordingly.
tion. A 0.1% solution is made from
10% of a 1% solution. Conclusion
• Formulas or compounding work-
Weighing accurately with no tolerance
sheets for solutions formatted in
is an unobtainable goal. The equip-
the, “weigh accurately, approx-
ment, at its best, is perhaps only accu-
imately…” manner can give greater
rate to around 1% of target weight
accuracy than fixed-quantity for-
without incorporating the human ele-
mulas. This means that when mak-
ment, which may increase this error.
ing a solution for use in production,
Because compounds frequently have
the compounder should record the
materials at concentrations of less than
exact weight of the target material
1% of the total formula, the use of
they have added to be diluted on
solutions appears to be justified. If we
the formula/worksheet. For ex-
can maintain an accuracy of 1% of the
ample, while making 100 g of a
target weight of both the solute and
10% solution, if the compounder
solvent there should be no detrimental
finds they have actually weighed
effect on the odor of the finished com-
out 10.15 g of the concentrated
pound.
material, they adjust the new total
These guidelines can help students
from 100 to 101.50 g, indicating
to plan formulations using solutions to
that the amount of solvent is to be
achieve consistent perfume quality
increased from 90 g to 91.35 g.
without the unnecessary inclusion of
A further example is provided in
expendable dilutions (e.g. 5% of phe-
Table 1.
nyl ethyl alcohol, a low-impact mate-
• Solutions should pass QC the same rial 10% in DPG, a relatively odorless
as any other compound. Strength and inert solvent) and ease the
is best determined in QC by GC or compounder’s burden slightly.
smelling the solution at 1% in etha-
nol and dropping the same number References
of drops onto smelling strips. Address correspondence to Stephen
Dowthwaite, PerfumersWorld.com, 111
• Laboratory use of solutions filled Prachachuen 37, Prachachuen Rd.,
from production-area stock bottles Bangsu, Bangkok, Thailand 10800.