We use Hydranal water standards. There are two kinds typically used. 1) 0.1 normal and 2) 1.0 normal.
The 0.1 normal administered at about 1mL should result in 100PPM (Parts Per Million) of moisture when measured. The acceptable result for this standard from the Karl Fischer titrator is +- 10%. So your Karl Fischer Titrator should produce a reading between 90PPM and 110PPM to be in the acceptable range. If it is, you know your Karl Fischer Titrator is performing correctly.
For the 1.0 normal everything is the same except for the standard should result in 1,000PPM and your acceptable range is smaller at +-3%. So your Karl Fischer Titrator should produce a reading between 970PPM and 1,030PPM.
I found this great video on Sigma Aldrich's site that shows this process (it also goes into some additional detail for conducting a water standard test). To see it go to:
http://www.sigmaaldrich.com/Area_of_Interest/Analytical__Chromatography/Video/HYDRANAL/water_standard_use.html
Hope this helps.
H.
We have a couple of ways to approach this application using a karl fischer titrator.
1. Use a Volumetric karl Fischer titrator; Volumetric is used where sample size is a little larger and the amount of expected moisture to be detected is higher (usually over 1.5% for example – not a rule, just a general guideline).
2. Use a Coulometric Karl Fischer titrator; Coulometric is used when a smaller sample size is used and the amount of expected moisture to be detected is lower (usually under 1% or 10,000ppm).
Both 1 and 2 above assume direct injection of the sample into the vessel. However, you can add an oil evaporator to either option above. The Oil Evaporator allows the operator to heat the oil and have nitrogen gas carry the H2O into the vessel where the moisture is measured. This keeps the vessel clean and should allow the operator longer use of their reagent before having to dump and refill the vessel with fresh reagent.
Regardless of the variety of your crude oil samples all of the above solutions work (in theory). Some are just more convenient than others, eg. Time to test, cleaning, etc.
The US military has been using the WBGT to determine appropriate activity levels in hot weather conditions for decades. The system, which uses different color flags to indicate the conditions, was developed by the Marines in the 1950s. The table below has the breakdown for each flag color.
|
Flag Color |
WBGT Index |
|
Green |
80-84.9 |
|
Yellow |
85-87.9 |
|
Red |
88-89.9 |
|
Black |
>90 |
Each level has guidelines for water intake and physical activity level for acclimated and unacclimated individuals.
To learn more about how the US Marines use the WBGT, click here.
On July 5th, a new workplace rule designed to protect workers from outdoor heat exposure will take effect in Washington State. This rule was passed on June 4 after six public hearings were conducted on heat stress and its causes. The hearings confirmed what officials already knew: working outside in hot weather is a health hazard. Over the past three years, 3 workers have died in Washington due to heat-related illness, and over 250 more have filed worker’s compensation claims for injuries directly resulting from heat-related illness in the past ten years. Washington officials hope that this law will decrease those statistics at a minimal cost to employers. The three requirements for employers with employees who work outside are to:
· Train employees and supervisors to recognize heat-related illness and what to do if someone has symptoms.
· On days when temperatures require preventive measures, increase the volume of water available to employees.
· Have the ability to appropriately respond to any employee with symptoms of illness.
The Wet Bulb Globe Thermometer (WBGT) is a tool perfectly suited to helping Washington State employers comply with this new law. This hand-held tool is used to estimate the effect of temperature, humidity, and solar radiation on humans and determine appropriate exposure levels to high temperatures. A WBGT index is commonly used as a guide for environmental heat stress to prevent heat stroke during physical exercise or while at work. Based on the index shown, employers can estimate the probability that a heat-related illness with occur and provide the appropriate amount of water available for the current weather conditions. For a video demonstrating the use of the WBGT, click here.
For more information on the new Washington State law, click
here.
From: Capt. Kara Escajeda CRDAMC Environmental Health Science Officer
(June 9, 2008) - Heat related injuries at Fort Hood Texas can result in as many as 225 people requiring medical care per year, primarily between May and September.
There may be up to 10 times that number that go unreported. Some of these injuries can lead to permanent damage to the brain and organs, and even result in death.
Heat injuries are completely preventable and the single most important prevention activity is proper training and awareness.
Education should include risk factors, early warning signs of an injury, treatment, weather monitoring, and control measures.
Strenuous events, especially those that are individually timed such as road marches, land navigation and physical training, are high risk events during the summer months.
Wearing MOPP gear, body armor, or working inside an armored vehicle are also times when you are more susceptible to an injury.
It is not just the elevated temperatures that you must be concerned with; it is the added effect of the humidity.
Humidity above 50 percent reduces your ability to cool your body through perspiration because it is not being evaporated.
That is why the Army states it is necessary to perform a Wet Bulb Globe Temperature (WBGT).
The WBGT measures radiant heat, humidity, temperature, and air movement which provides an index to determine recommended work/rest cycles as well as the amount of water that should be consumed.
Heat injuries in the 70s are common because the humidity is not taken into consideration.
Also keep in mind that activities prior to a strenuous event are just as important as those during the event.
For instance alcohol consumption 24 hours prior to an outdoor activity increases the loss of fluids and reduces your body’s ability to tolerate heat.
Decreased rest is a serious risk factor for heat stroke so ensure you get plenty of sleep in the days leading up to an event.
When you are fatigued, your body is less efficient at regulating your body temperature.
Proper hydration 24 to 48 hours prior to a strenuous outdoor event can reduce the risk of injury. You can tell if you are properly hydrated by the color of your urine.
If your urine is dark or you have not urinated then you have not been drinking enough. You are striving for a light yellow color.
Equally important to hydration, is ensuring that you eat enough meals to replace salts.
Drinking too much water and not eating enough can be fatal.
That is why it is important to not follow a low calorie diet while training in a hot environment, but instead try to eat meals in smaller portions throughout the day.
Energy drinks, such as Red Bull, have become readily available and a common choice for a pick me up.
These drinks are okay in moderation, but do not consume them prior to a strenuous event such as Physical Training.
Your heart rate and blood pressure are already elevated from the physical exertion and the extra caffeine from the drink will make it even harder on your body.
Mild Heat Injury Signs
Dizzy
Headache
Nausea or Vomiting
Feeling tired or Weak
Unsteady Walk
Muscle Cramps
Severe Heat Injury Signs
Confused behavior
Combative
Passes out
* Treatment: Cool body and Call for help
Risk Factors
-- Prior heat injury
-- Overweight
-- Poor fitness
-- Not adequately acclimated
-- Taking certain medications
-- Use of alcohol within 24 hours
-- Skin disorders or sunburn
-- Minor illness (sore throat, fever, cold)
-- Over 40 years old
Medication that increase risks
for heat injuries
-- Antihistamines
-- Some cold medicines
-- Blood pressure medication
-- Some narcotics
-- Psychiatric medication
There are multiple methods of moisture determination, including loss on drying, Karl Fischer titration, piezoelectric sorption, spectroscopy, and chilled mirrors among others. However, it is advantageous to use Karl Fischer (KF) titration in moisture analysis for the following reasons:
- It is highly accurate and precise.
- KF is specific to water determination. This specification is different from the other popular moisture analysis method, loss on drying (LOD), because LOD can detect the loss of any volatile substance. However, this specification is advantageous because it allows KF titration to work independent from volatile substances present in the sample
- The process does not require large samples, which is especially true with coulometric Karl Fischer titrators.
- It does not require much time to perform an analysis since the samples are easy to prepare and the analysis itself is short in duration.
- The method has a nearly unlimited measurement range (from 1ppm to 100%).
- Karl Fischer titration can determine the moisture content of a sample in any state, whether it is a solid, liquid, or gas.
The above advantages show that Karl Fischer titrators are versatile and efficient scientific instruments to use for moisture analysis.
A quick reference:
1.0% (0.01) moisture = 10,000PPM
0.9% (0.009) moisture = 9,000PPM
0.8% (0.008) moisture = 8,000PPM
0.7% (0.007) moisture = 7,000PPM
0.6% (0.006) moisture = 6,000PPM
0.5% (0.005) moisture = 5,000PPM
0.4% (0.004) moisture = 4,000PPM
0.3% (0.003) moisture = 3,000PPM
0.2% (0.002) moisture = 2,000PPM
0.1% (0.001) moisture = 1,000PPM
0.09% (0.0009) moisture = 900PPM
etc.
0.05% (0.0005) moisture = 500PPM
etc.
0.01% (0.0001) moisture = 100PPM
Also,
PPM= water detected (in micro grams)/ sample size (in grams)
Understanding how these relationships and measurements relate is very useful when determining testing methods you may want to employ. As a general rule Karl Fischer (some refer to it as "water by karl fischer" or "Karl Fischer titrator/titration") is ideal when you need to measure moisture at these levels with accuracy in the PPM (parts per million) range.
Hope this was helpful.
-H
From Wikipedia, the free encyclopedia
This article is about volumetric titration.
In medicine, titration is the process of gradually adjusting the dose of a medication until the desired effect is achieved. Not to be confused with Tetration.
Titration setup: the titrant drops from the burette into the analyte solution in the flask. An indicator present then changes color permanently at the endpoint.
Titration is a common laboratory method of quantitative/chemical analysis that can be used to determine the concentration of a known reactant. Because volume measurements play a key role in titration, it is also known as volumetric analysis. A reagent, called the titrant, of known concentration (a standard solution) and volume is used to react with a solution of the analyte, whose concentration is not known in advance. Using a calibrated burette to add the titrant, it is possible to determine the exact amount that has been consumed when the endpoint is reached. The endpoint is the point at which the titration is complete, as determined by an indicator (see below). This is ideally the same volume as the equivalence point - the volume of added titrant at which the number of moles of titrant is equal to the number of moles of analyte, or some multiple thereof (as in polyprotic acids). In the classic strong acid-strong base titration, the endpoint of a titration is the point at which the pH of the reactant is just about equal to 7, and often when the solution permanently changes color due to an indicator. There are however many different types of titrations (see below).
Many methods can be used to indicate the endpoint of a reaction; titrations often use visual indicators (the reactant mixture changes colour). In simple acid-base titrations a pH indicator may be used, such as phenolphthalein, which becomes pink when a certain pH (about 8.2) is reached or exceeded. Another example is methyl orange, which is red in acids and yellow in alkali solutions.
Not every titration requires an indicator. In some cases, either the reactants or the products are strongly coloured and can serve as the "indicator". For example, an oxidation-reduction titration using potassium permanganate (pink/purple) as the titrant does not require an indicator. When the titrant is reduced, it turns colourless. After the equivalence point, there is excess titrant present. The equivalence point is identified from the first faint pink colour that persists in the solution being titrated.
Due to the logarithmic nature of the pH curve, the transitions are, in general, extremely sharp; and, thus, a single drop of titrant just before the endpoint can change the pH significantly — leading to an immediate colour change in the indicator. There is a slight difference between the change in indicator color and the actual equivalence point of the titration. This error is referred to as an indicator error, and it is indeterminate.
Types of titrations
Titrations can be classified by the type of reaction. Different types of titration reaction include:
• Acid-base titrations are based on the neutralization reaction between the analyte and an acidic or basic titrant. These most commonly use a pH indicator, a pH meter, or a conductance meter to determine the endpoint.
• Redox titrations are based on an oxidation-reduction reaction between the analyte and titrant. These most commonly use a potentiometer or a redox indicator to determine the endpoint. Frequently either the reactants or the titrant have a colour intense enough that an additional indicator is not needed.
• Complexometric titrations are based on the formation of a complex between the analyte and the titrant. The chelating agent EDTA is very commonly used to titrate metal ions in solution. These titrations generally require specialized indicators that form weaker complexes with the analyte. A common example is Eriochrome Black T for the titration of calcium and magnesium ions.
• A form of titration can also be used to determine the concentration of a virus or bacterium. The original sample is diluted (in some fixed ratio, such as 1:1, 1:2, 1:4, 1:8, etc.) until the last dilution does not give a positive test for the presence of the virus. This value, the titre, may be based on TCID50, EID50, ELD50, LD50 or pfu. This procedure is more commonly known as an assay.
Particular uses
• As applied to biodiesel, titration is the act of determining the acidity of a sample of WVO by the dropwise addition of a known base to the sample while testing with pH paper for the desired neutral pH=7 reading. By knowing how much base neutralizes an amount of WVO, we discern how much base to add to the entire batch.
• Titrations in the petrochemical or food industry to define oils, fats or biodiesel and similar substances. An example procedure for all three can be found here: [1].
• Acid number: an acid-base titration with colour indicator is used to determine the free fatty acid content. See also: pH of fatty acids.
• Iodine number: a redox titration with colour indication, which indicates the amount of unsaturated fatty acids.
• Saponification value: an acid-base back titration with colour indicator or potentiometric to get a hint about the average chain length of fatty acids in a fat.
I contacted the author and he gave me permission to post the article here.
Subject: Measuring Coffee Strength With A Brix Meter
- Alan Alder, Palo Alto CA.
Do you enjoy tinkering with grinding and brewing techniques? Do you have about $270 to blow on your coffee hobby? If not, this isn’t for you. But if so, read on.
While developing the AeroPress, I needed a method to measure brew strength. I first tried the SCAA Total Dissolved Solids (TDS) meter but found the results inconsistent. I called SCAA and discussed it with their Technical Director, Joseph Rivera. I mentioned that I was an electronics engineer and thought that the TDS meter, which is simply a conductivity meter, was too sensitive to small variations in saline content of the water or the finished brew. Joseph agreed and said that he had heard that someone was using a Brix meter.
A Brix meter measures index of refraction and is normally used to measure sucrose level of liquids such as juice or wine. A Google search for Brix and coffee measurement came up empty, but I decided to give it a try and bought a $270 Atago PAL-1 digital Brix meter. It turned out to be the answer to my needs.
To measure brew strength with a digital Brix meter you put a few drops of brew on a small glass window and press the button. Voila! A reading appears. No calibration baths or other annoyances. It fits in my pocket and I can take it from my lab to a coffee shop whenever I wish.
After using Brix for about a year, I took it to the SCAA Convention in Seattle last April and showed it around. One of the first people I showed it to was Joseph Rivera. A few months later, he bought one himself and is now a confirmed Brix user. He also told me recently that his dehydration instrument verified that Brix is far more accurate than the old conductivity meter they sell.
Another person I showed it to was Randy Pope of the Bunn Technology Center. Randy pulled out his own Brix meter and told me that he’d been using it for eleven years and that it was very accurate. He also shared measurements he’d made to correlate Brix to Total Dissolved Solids as measured with his dehydration instrument. He found that 0.85 x Brix equals the percent Total Dissolved Solids (TDS).
The SCAA recommends 1.25 percent TDS for ordinary brewed coffee. That corresponds to 1.47 Brix, which the meter rounds to 1.5. There is no standard for espresso, but I’ve measured hundreds of shots and find that most are in the ranges from about 3.4 for pod and capsule machines to about 7.5 for professional pulls. Here are some measurements that I’ve made:
1.5 Krups drip brewer with paper cone filter
2.1 Brewed coffee at Peet’s – Los Altos, California
3.4, 3.6 Nespresso capsule brew
3.7 Victoria House concentrate
4.8 Starbuck's, Los Altos
4.4 Filtron cold-brewed concentrate SCAA booth
4.9 Solis automatic at Baratza SCAA booth
5.2 Ken Davids' Saeco Vienna (Summer 2004)
5.3 Ken Davids' Saeco Vienna July 25, 2005
5.9 An old Italian lever machine
5.6 Rancillo booth at SCAA
7.3,7.4 Pasquini Riviera machine
7.5 Peet's, Palo Alto, California
20.6 Cafe' Vivace, Seattle
The last reading is unusually high and the product of espresso-guru David Schomer, who clearly likes a very intense shot.
My own taste buds prefer about 7.5 for straight espresso but I make it stronger when making a shot that will go into a latte. Of course I brew my shots in an AeroPress, which can make any Brix I want, even up into the twenties.
Here are two tips on Brix measurement of coffee:
1. The meters is temperature sensitive. It can take about a minute for the sample to cool enough to give a stable reading.
2. Brix is primarily a method of measuring sucrose level, so there must be absolutely no sugar in your sample.
After measuring the Brix level of hundreds of samples, I developed this formula:
Brix is approximately equal to K times (coffee weight) / (water weight)
K equals about 23 for an AeroPress using fine drip grind and 175F water -- which is everybody’s favorite AeroPress temperature.
K increases to about 27 for a conventional espresso machine which uses both finer grind and hotter water.
It’s easy to weigh the input coffee and input water with an AeroPress, but more complex with a conventional espresso machine. Barry Jarrett asked me how I do that. Here is my answer:
Weigh the empty portafilter.
Add and tamp coffee, weigh it again and subtract empty portafilter weight to get dry coffee weight.
Weigh the output cup.
Pull the shot.
Weigh the cup of brew and subtract empty cup weight to get brew weight.
Weigh the portafilter containing the damp puck and subtract empty portafilter weight to get wet puck weight .
Input water weight = brew weight + wet puck weight - dry coffee weight.
You can also use a formula based on coffee weight / brew weight. That's simpler with a conventional espresso machine and the formula is about:
Brix ~ 18 times (coffee weight) / (brew weight)
I also find Brix to be an excellent tool for evaluating grinders. If the grind isn’t as fine as claimed, the brew will be weak and the Brix low. All the cheap burr grinders I’ve tested fell far short of the formula, even on their finest setting.
As I said in the beginning, Brix isn’t for the casual barista. But if you’re a Mark Prince, or Barry Jarrett or David Schomer, after you try Brix you’ll wonder how you ever got along without it.


If you use water or chemicals, you probably need reliable pH measurement for
• Quality Control
• EPA compliance
• Safety
• Maximum productivity
Water treatment plants, wastewater treatment plants,
chemical plants, paper mills, metal processing plants,
textile mills, automotive plants, food processing
plants, power plants and more need to measure and
control pH.
The speed or rate of chemical reactions and degree of
solubility are directly related to pH. Living organisms
survive in a very specific pH range.
So what is pH?
pH represents the amount of available Hydrogen ions
in a solution. It is defined as the negative log of the
activity of Hydrogen ions. The scale ranges from 1 to
14 with 7 being neutral.

Even though this measurement is heavily relied upon
there is little attention paid to the acceptable toler-
ances for a properly functioning pH electrode. In fact,
many do not realize that the typical electrode life is
between 6 months to 1 year. How long an electrode
actually lasts is dependent upon its maintenance, types
of solutions measured, and the temperatures. It is the
intention of this article to explain a method to determine
if an electrode is operating within acceptable tolerances
in an effort to avoid potentially erroneous measurements.
The pH measurement of a solution is based upon the
potential developed by a pH electrode and can be
determined by the Nerst equation:

Where [E obs] is the observed potential generated; [Ec] is
the sum of all the constant potentials, R is the gas con-
stant, T is the temperature in K, and F is Faraday’s
constant.
Theoretically according to the Nerst equation, at 25°C
an electrode in pH 7.0 solution will generate 0 mV
potential and for each pH unit away there will be an
increase of 59.16 mV. A pH of 4.0 will generate
+177.48 mV while a pH of 10.0 will generate –177.48
mV. The potential generated is dependent on the tem-
perature of the solution. Figure 1 shows the impact of
temperature on what mV will be observed at various
pH values. Note that the impact of temperature is
greater at the extremes. Most pH meters have automat-
ic temperature compensation (ATC) to correct for this
effect.

Electrodes in use differ from the theoretical maxi-
mums obtained by the Nerst equation. Differences can
be due to many factors including manufacturing toler-
ances, electrode aging, conditioning, and cleaning.
The calibration process allows for the standardization
of the electrode to compensate for these factors but
does so with little regard to its optimal functionality.
A method to determine the status of an electrode is to
look at the mV readings rather than pH. From a mV
reading a slope percentage can be calculated.
Electrodes with slope percentages of 90-105% are
generally said to be in good condition. It is important
to perform the analysis with fresh uncontaminated
buffers. It is always important to clean the electrode
and store it properly when not in use. The following
calculations described are based on using buffers that
are at ambient room temperature of 25°C.
Calculating the slope percentage is relatively easy to
do. First, the mV generated from an electrode in pH
7.0 buffer is recorded. This reading is known as the
offset and should fall within +/- 25 mV. Readings out-
side this range indicate a problem. Second, the mV
reading generated by the electrode in a pH 4.0 or 10.0
buffer is recorded. This reading is known as the slope
adjustment and generally should fall between +/- 150
mV to +/- 186 mV. Again outside these ranges indi-
cates a problem. To calculate the slope percentage the
offset reading is subtracted from the slope reading.
This number is then divided by the theoretical maxi-
mum +/- 177.48. To change to a percentage simply
multiply by 100. Acceptable slope percentages should
fall within the 85% to 105% range.
Example 1:An electrode in pH 7.0 buffer generated
15 mV while in pH 4.0 buffer it generated +175 mV.
The net difference of +160 mV is then divided by
+177.48 mV. The result, 0.901 is then multiplied by
100 to give a slope percentage of 90.1%. Figure 2
shows a graph of this line and compares the change to
an electrode operating at the theoretical maximum of
59.16 mV/pH unit with the same 15 mV offset.

Again, an electrode having a slope percentage of 90%
is generally thought to be in good condition. It is still
possible to have a good slope percentage but not have
an electrode within acceptable tolerances.
Example 2:An electrode in pH 7.0 buffer generated
75 mV while in pH 4.0 buffer it generated +235 mV.
The net difference of +160 mV is then divided by
+177.48 mV. The result, 0.901 is then multiplied by
100 to give a slope percentage of 90.1%.
Note that the offset and slope values are outside the
acceptable ranges stated earlier but still generate a
good slope percentage. Graphically there is a complete
shift of line of 60 mV and can be seen in figure 3.

If this shift is due to an electrode being “dirty”then
this can lead to a potential problem. As the contami-
nants come off the electrode during use the electrode
characteristics will change. This change will result in
a calibration that is no longer valid and any readings
obtained will be inaccurate.
How do you determine the reliability of your pH
electrodes?
Hanna instruments manufactures a microprocessor-
based instrument that analyzes the mV generated by
the offset and slope measurements. The bench-top
HI221 and HI223 are designed to alert you to the
condition of the electrode during the calibration
process. These indicators include probe condition,
response time, “clean”electrode, and contaminated
buffers. Built in GLP features allow the user to review
calibration data including time, date, buffers used, and
the slope of the electrode. Calibration time-out feature
can be enabled to notify the user when it is time to
recalibrate. The HI 221 can log up to 100 points and
has a resolution/accuracy of 0.01/+0.01 pH. The HI
223 can log up to 500 measurements and has a resolu-
tion/accuracyof 0.001/+0.002 pH. Both can download
data to a computer through an RS232 connection.
Contributed by
Paul Fabsits,
Hanna
Instruments
All and all the Du Nouy ring is a standard in the industry whether you are using a manual tension meter or using a digital tension meter.
I have not used a digital tension meter ...yet, but have seen a video of one on you tube:
You Tube Video - Digitial Tension Meter (New window)
notice in the video your choice of Du Nouy ring or Wilhemy plate,
Stew
Well basically, moisture testing using the karl fischer method is a standard in the industry that measures down to the Parts per million (PPM) level. The theoretical accuracy is down to 1 part per million level. I say theoretical because usually any variance is due to atmospheric conditions and operator repeatability. Specifically, and for this example, "coulometric" Karl Ficsher is best when you are using a small sample and expect and are trying to measure less than 1% (1%moisture =10,000PPM) of water (moisture/humidity) in your sample. [Note: there is a volumetric Karl Fischer method vs. coulometric Karl Fisher method but for this discussion I am speaking from the coulometric Karl Fischer standpoint]
With this in mind,
A. If you are testing a liquid sample you only have to use the karl fischer titrator and directly inject the liquid sample with a syringe (usually around 1mL) into the vessel.
B. If you are testing a solid sample (that cannot be "broken down sufficiently with solvents like Xylene for example) you will use both the karl Fischer AND an evaporator oven. The evaporator oven heats up the sample (usually the sample size is less than 1gram...we typically might use 1/10th of a gram). The evaporator is connected with a nitrogen gas source that is used to deliver the moisture via a heater tube on the evaporator into the titration vessel.
To see an actual demonstration of the Karl Fischer and the evaporator oven during an actual test please go to the link below and watch the short 2 to 3 minute video.
http://www.scientificgear.com/Karl-Fisher-titration/Karl-Fisher-Accessories/Evaporator-KF-610-series
To be sure there are many more things I could mention but this is a high level summary of the two approaches.
Hope this helps.
H.
Some tension meters just measure surface tension, where as the ring is only pulled up from the liquid, other tension meters can also measure downward forces ( interfacial ) which can employ a du nouy ring or be fitted with a wilhemy plate.

