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Do ketones affect moisture readings in Karl Fischer Titration?

By Hank Levi on Mon, Nov 13, 2023 @ 03:40 PM

Yes, ketones can potentially affect moisture readings in Karl Fischer titration. This is because ketones can react with the methanol in common Karl Fischer reagents, forming acetals, which also react with the reagent and produce water. This additional water is then titrated and can cause the moisture reading to be too high. In order to avoid this, it is important to ensure that the titration cell is cleaned thoroughly after each analysis to remove any traces of ketones that may be present. If traces of ketones are left in the cell, it can cause erroneous readings and affect the overall accuracy of the moisture measurement.  Additionally, there are some specialty reagents, Coulomat AK and Coulomat CGK,  that can be used to help limit this side reaction....and also you have the option of using a Volumetric Karl Fischer Titrator to get around this problem.

 

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Benefits of Using Karl Fischer Moisture Titration vs. Other Methods

By Hank Levi on Thu, Jun 22, 2023 @ 04:33 PM

Accurate measurement of moisture content is essential to ensure the quality and consistency of your products. There are several methods available for measuring moisture content, but one of the most reliable and accurate methods is Karl Fischer moisture titration.

Karl Fischer moisture titration is a widely used method for measuring moisture content in a variety of materials, including solids, liquids, and gases. This method is based on the reaction between water and a Karl Fischer reagent, which produces a measurable electrical signal. The amount of water present in the sample can be calculated from the electrical signal, providing a precise measurement of moisture content.

One of the main benefits of using Karl Fischer moisture titration is its high accuracy. This method can detect moisture levels as low as 0.001%, making it ideal for applications where even small amounts of moisture can have a significant impact on product quality. In addition, Karl Fischer moisture titration is highly selective, meaning that it only reacts with water and not other substances in the sample. This makes it an excellent choice for measuring moisture content in complex mixtures.

Another advantage of Karl Fischer moisture titration is its versatility. This method can be used to measure moisture content in a wide range of materials, including pharmaceuticals, food products, and industrial chemicals. It can also be used to measure moisture content in gases, making it an essential tool for applications such as natural gas processing and semiconductor manufacturing.

Compared to other methods for measuring moisture content, Karl Fischer moisture titration is also relatively fast and easy to perform. The titration process can be automated, reducing the risk of human error and increasing efficiency. This makes it an excellent choice for high-throughput applications where speed and accuracy are essential.

Share this with associates who may find  an analysis of Karl Fischer titration useful.

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Introducing our technical Web Helpers!

By Hank Levi on Mon, Nov 23, 2020 @ 01:58 PM

Hello!  Please meet our new Web Helpers!  Moisture Elle, Karl Fischer, Shaker Sam, Terri Tenso, and Vivian Visco!  Each of our helpers will provide technical information ranging from general topics to more in-depth discussion pertaining to; Moisture testing, Karl Fischer Titration, Particle Size Analysis, Surface Tension, and Viscosity.

 

 

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How an oil evaporator works with a Karl Fischer Titrator

By Hank Levi on Mon, Aug 26, 2019 @ 11:13 AM

Evaporators configured for use with Karl Fischer moisture testers can provide added benefit when testing for moisture in samples that are not easily solubilized in the titration cell.  In some cases even if it's possible to solubilize the sample in the titration cell you may find that it is better to use an evaporator to improve repeat testing by keeping the cell clean.  While traditonal Karl Fischer moistutre testing is performed using a direct injection method where a syringe and needle is used to introduce the liquid sample into the titration cell, the use of evaporators follow a different approach. 

Within the evaporator family there are SOLIDS EVAPORATORS that can range from 0 to 300 degree C as well as high heat solids evaporators that can range from 0 to 1,000 degree C. 

A typical OIL EVAPORATOR will have a range from 0 to 300 degree C. 

Solids evaporators will typically be used to measure moisture in these types of samples:

  • plastic pellets (pte, etc)
  • plastic parts (you can cut into smaller pieces with a pair of scissors)
  • paper material (transformers)
  • thick grease samples
  • thick petroleum based samples like heavy paints, etc
  • and the list goes on

Oil evaporators will generally be used when working with heavy crude oil samples with high turnover testing (keeping the cell clean).

In this video we will discuss and show how the oil evaporator works with a Karl Fischer Titrator.

 

Talking points include:

  • Karl Fischer Titrator
  • Oil Evaporator
  • Base Oil
  • Bubbler Tube
  • Nitrogen Gas Source
  • Regulator
  • Thermocouple
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What happened to Hydranal Karl Fischer Reagents?

By Hank Levi on Sun, Nov 05, 2017 @ 08:12 PM

There has been some confusion in the market place when it comes to purchasing Karl Fischer reagents and water standards.  Some of you who have traditionally ordered the Hydranal brand from Sigma Aldrich (and it's channel partners and dealers) are discovering now that the Karl Fischer reagents and waters standards are slightly different - If you order them from Sigma Aldrich.  The names on the bottles are kind of the same, but not exactly.

milliporesigmalogo.png

Some background - what happened to Sigma Aldrich

As many people know Sigma Aldrich for many years handled the Hydranal line of Karl Fischer Reagents and water standards.  Recently (within the past year and a half or so), a company called EMD who controls the other Karl Fisher reagent line called Aquastar purchased Sigma Aldrich.  As a result of this transaction Sigma Aldrich is now part of another company and is referred to as MilliporeSigma.The Sigma Alrdrich you used to know no longer provides the Hydranal brand but intstead now offers the Aquastar line of Karl Fischer Reagents and water standards.

What happened to the Hydranal brand of Karl Fischer reagents?

honeywelllogo.jpgA well-known company called Honeywell purchased and now controls the Hydranal line of Karl Fischer Reagents.  You can still order Hydranal brand coulometric Karl Fischer reagents and volumetric Karl Fischer reagents via Honeywell and it's channel partners and distributors.

What does this mean to you and how might this effect you?

As you can imagine this has triggered a lot of phone calls with questions from end-users to purchasing agents with questions like:

  • Are these reagents the same?
  • Can I use these reagents interchangeably?
  • What are the differences?
  • Hydranal vs. Aquastar?

Here's what we know

As a manufacturer and distributor of coulometric Karl Fischer titrators and volumetric Karl Fischer titrators for many years, we have worked with both the Aquastar and Hydranal brands extensively.  We are not here to tell you one is better than the other.  We can tell you that different model Karl Fischer titrators seem to work differently depending on the brand of Karl Fischer reagent used.  It might simply be an operators familiarity with working with one brand vs. the other or it might be because a specific application just works better with a certain Karl Fischer reagent.  

-While the design is that either of these brands should work we find subtle differences in chemistry-  

Are there any real key chemical differences between Hydranal and Aquastar?

To be fair we have not reached out to Aquastar for their perspective yet (we will - and update this post).  From the Hydranal technical center we have obtained some information about what they see as strengths in the Hydranal brand and some differences with the Aquastar brand.  Here are a few notable points:

1. Different performance.  Yes they do perform differently.

2. Different solvents are used.  Example:  Aquastar Combititrant is a copy of the old version of Hydranal Composite 5 where there was no 2-Methylimidazole.  Without 2-Methylimidazole, you can have reagent crystalization and stability issues.

3. Co-solvents are optimized in Hydranal.  Too much Chloroform can mess up the stoichiometry

4. Hydranal coulometric reagents are more unique

  • Hydranal has more buffering capacity
  • Larger volume of samples than Aquastar

5. Hydranal is very precise, convenient and consistent

As mentioned above we hope to get some additional information on the Aquastar line so we can share with you their strengths and differences.  In the meantime we hope this information has been helpful.

If you have any questions or would like to compare the reagents you currently use with the "other" brand just let us know.  We can provide a cross reference for all of the Karl Fischer reagents by brand and product.

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As always, we hope this information is helpful.

 


 



 

 

 

 

 

 

 

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How to find Bromine number and index with a Karl Fischer Titrator

By Hank Levi on Sun, Apr 10, 2016 @ 08:47 AM


WHY DO WE CARE ABOUT BROMINE NUMBER AND BROMINE INDEX ANYWAY?

The degree of unsaturated hydrogen carbide (Hydrocarbon) in oil and petroleum products is indicated by Bromine number or index. Hydrocarbons containing between 6 and 10 carbon molecules are the primary components of most fuels where the process of burning them produces energy. Saturated hydrocarbons are defined by molecular structure and are defined as Alkanes.  Alkanes are the basis for petroleum fuels.  Unsaturated hydrocarbons are also defined by their molecular structure and produce less energy when burned than do saturated hydrocarbons.  Mathematically it therefore requires a greater quantity of unsaturated hydrocarbons to be burned to equal the same amount of energy produced by burning the same amount of saturated hydrocarbons.  An un-friendly environmental side effect of burning hydrocarbons is the creation of carbon dioxide.  So from an environmental standpoint you could say we prefer the lesser of two evils and prefer to burn saturated hydrocarbons vs. unsaturated hydrocarbons. For these reasons alone it would make sense that we would want to measure and quantify these hydrocarbons. 

 

HYDROCARBONS AND SOME OF THEIR USES

NAME USES
Methane Fuel in electrical generation
Ethane Chemical applications
Propane Heating and cooking
Butane lighters and aerosol
Pentane Lab & production of polystyrene
Hexane Glue
Heptane & Octane Major contributor to gasoline
Nonane

Diesel fuel

Decane

Jet fuel, gasoline and diesel

 

Although the test method ASTM2710 describes the use of an automatic potentiometric titrator the coulometric Karl Fischer method is easier to perform (see ASTMD1492-08e1).  



<BROMINE NUMBER AND INDEX BY COULOMETRIC KARL FISCHER TITRATION>

Bromine number :The amount of bromine (unit: g/100) consumed in 100g sample.

Bromine index :The amount of bromine (unit: mg/100) consumed in 100g sample.

 

<PRINCIPAL OF MEASUREMENT>

The unsaturated hydrogen carbon reacts with bromine as follows: R-CH=CH-R+Br2R-CHBr-CHBr-R- (Eq. #1)

In coulometric titration, bromine is generated by electrolysis of anolyte containing bromine ion:  2Br-Br2+2e- (Eq. #2)

 

When generated bromine is consumed according to Eq. (#1), the electrode detects bromine consumption, and continues generating bromine according to Eq. (#2).

Such bromine is generated in proportion to the electricity determined by Faraday’s Law. From Eq. (#1), Bromine reacts with coupled C=C evenly (1:1). ==>Thus, one mol of bromine(159.8g) is equivalent to 2 96500 coulomb, which means 1.2 coulomb/1mgBr2.

Based on the above principle, the electricity consumed in electrolysis is converted to the exiting bromine.

 

Special notes to obtain correct measurement results:

  1. Replace anolyte and catholyte reagent often (daily).
  2. When anolyte turns to white color replace it with new anolyte.
  3. Over use of anolyte and catholyte and not replacing it can cause results to be higher than expected.
  4. Do not share Bromine titration cell with a moisture titration cell

 Download a copy of this method

Step 1: Preparation of Reagents

Prepare the reagents and samples for measurement of bromine number and bromine index.

Use the following reagent for measurement of bromine number or index:

Anolyte Reagent: Mixture of Acetic acid (high grade) 600mL; Methanol (high grade) 260mL; 1M-Potassium bromide solution 140mL. Blend it well and use 100mL each time.

Catholyte Reagent: 0.2M-Potassium chloride solution. Use 5mL each time.

Check Solution:  0.05Wt-Cyclohexene toluene mixture (Approx. 93 ~ 102mgBr2/100g). Theoretical value is calculated by the below formula:

theoreticalbrominevalue.png

 

Step 2: Prepare Reagent for testing

Refer to the below chart for sample size:

Bromine index (mg/100g)  Sample Size (g) 

 Below 10

10 ~ 50

50 ~100

100 ~ 200

More than 200

 10 ~ 15

5 ~ 10

3 ~ 5

1 ~ 3

~ 1

For bromine number, a sample is diluted with toluene to Bromine number 0.2 (g/100g), and approximately 1g is used for measurement. Calculate the toluene to be used for diluting to Bromine number 0.2 (g/100g) with the following equation:

anotherbromineformula.png

Obtain the dilution coefficient in advance according to the following equation:

Brominedilutioncoefficient.png

 

Step 3: Measurement Procedure

Measure Bromine Number and Bromine Index

  1. Discharge 20 100μL check solution into the electrolysis cell, and press [Pre-titr.*] key.

  2. After pre-titration is finished, press [Sample*] key to enter sample name, its ID and size, and enter the dilution coefficient (D) .
    Press [MENU/HOME*] to Main display.

  3. Press [Start] key, and discharge the sample into the cell. Again press [Start*] key for titration to start.

  4. After titration is over, the measurement results appear on display with printout when a printer is connected.

*Note that different Karl Fischer Titrator Models will have different button commands.  The MKC-710 series coulometric Karl Fischer titrators come standard with pre-programmed setup for running Bromine and follow the above button commands.

We hope this information helps you get started.  If you have any questions or would like some help please contact us by clicking on the button below.

Download a copy of this method 

 

 

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How to test for moisture in Jet Fuel Oil using a Karl Fischer titrator

By Hank Levi on Mon, Sep 21, 2015 @ 03:15 PM


From start to finish watch this short video to see how a sample of Jet Fuel Oil is tested for water content using a karl Fischer Titrator. For this training video we use:

  1. The Aquapal III coulometric Karl Fischer Titrator (setup as a dual reagent configuration)
  2. Reagents; Anolyte is coulomat AG and the catholyte is coulomat CG
  3. A 4-place analytical balance SA-210
  4. And a disposable syringe and disposable needle

In this video you will see the steps for running a test successfully including how to:

  1. Extract your sample into the syringe
  2. How to weigh your sample and tare the balance
  3. How to inject a sample properly
  4. How to input the sample weight and obtain a final result

 

Find out more about the Aquapal III

We hope you found the video helpful and informative!  If you think a colleague could benefit from this please share it with them!  Click on the twitter button to automatically share this video!

Tweet: How to test for moisture in Jet Fuel Oil using a Karl Fischer Titrator http://bit.ly/1NJ8If4"How to test for moisture in Jet Fuel Oil using a Karl Fischer titrator"


 

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Karl Fischer Glassware and reagents 101

By Hank Levi on Mon, Sep 21, 2015 @ 01:53 PM

Many people use coulometric Karl Fischer Titrators to measure low level moisture at the part per million (PPM) level.  When it's time to start testing it's critical to have an understanding of how to:

  1. Properly identify the glassware components
  2. Assemble the glassware
  3. Identify the reagents  (anolytes and catholytes)
  4. Introduce the reagents required by the instrument and the sample being tested 

Once you have these concepts down you will have a strong working knowledge of how a Karl Fischer Titrator works and how to trouble shoot future problems.  Watch this short training video to learn more.

Find out more about the Aquapal III

If you found this information helpful please share this with your colleagues!  Just click on the tweet this button.

 Tweet: Karl Fischer glassware & reagents 101: properly identify glassware components, assemble glassware & identify reagents http://bit.ly/1Qvwv1v "Karl Fischer Glassware and reagents 101: Properly identify the glassware components, Assemble the glassware and Identify the reagents"


We hope you find the training video helpful!
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Karl Fischer Glassware and Reagents 101: How to setup.

By Hank Levi on Wed, Jun 17, 2015 @ 10:53 PM

Karl Fischer Glassware and Reagents 101:  How to setup.

 Screen_Shot_2015-06-17_at_11.16.04_PM

It seems sometimes we overlook the obvious and forget to explain some of the most basic concepts.  Sorry about that.  So we thought it might be a good idea to show how Karl Fischer Glassware is setup and how we introduce or "charge" the vessel with reagents.  We hope you enjoy this short video tutorial!

 

 Find out more about the Aquapal III

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Review of KEM's new titration line

By Hank Levi on Tue, Jun 09, 2015 @ 04:11 PM


Review of KEM's new titration line 

AT-710S_M Automatic Titrator

I don't know about you but I have to admit that I enjoy learning about new technology.  Whether it's smart phones, cars, or kitchen appliances I think it's fun to find out about how a product has changed (hopefully for the better). For the most part a lot of consumer products see a change or upgrade about once every year. This is not really the case for titrators where maybe it's only every 6 to 8 years before we see a new generation unveiled.  I guess that's why I thought maybe it would be a good idea to take a look at this new 710 series that came out in February 2015.  I haven't actually ever written a "review" before so I decided to start by comparing what I know about some of the current titrator models and identify the things that pop out with the new titration line.   Here are my observations and comments.


  

1. There are now three model levels; entry, mid-level, and flagship within each category (volumetric Karl Fischer, coulometric Karl Fischer, and automatic potentiometric titrator) 

Find more Coulometric Karl Fischer Titrator information

My comment: I like the scale of the models as it can be helpful for those with varied budgets and needs.  I like the concept that you can start with getting only the basic model at first and then later bring in the flagship model and tie them all together into one system.  It will be interesting to see how people approach these options and whether the ability to expand a system is desirable or not.
710_series_titrator_with_2_burettes

2. All of the automatic titrators now can accommodate two burette drives

 AT-710 AutomaticTitrator information

My comment: The automatic titrators come with one burette drive but being able to add a second burette drive allows an operator to run two separate titrations (titrants) without having to use an automatic piston burette.  Historically most titrator manufacturers offered only a single burette drive but it seems like this is changing.  It's kind of a big deal for those who run two different titrations and don't want to purchase an automatic piston burette.  I like this new capability.

3.  A new burette design for the automatic titrators and volumetric Karl Fischer titrators.

SmartBuretteUnit

My comment: The burettes appear they will be easier to store and swap as the titrant bottle, burette and nozzles all go together as one smaller unit.   The burettes are now "smart" burettes and can store all of the reagent information within the head of the burette.  I like this.

Learn more about Volumetric Karl Fischer Titration

4.  More Input/Output options for operators to move  and store data.  I/O options include LAN connectivity/URL, USB hubs, USB thumb drive ports, .CSV file format, .PDF file format, barcode readers, foot switches, and keyboards.710seriesUSB

My comment:  More technology is built into these units. I think it was overdue so I am glad to see it finally arrive.

AT710_w_propeller_or_magnetic_stirrer

5.  Automatic Titrators now come with a propeller stirrer by default but can swap for a magnetic stirrer instead.

My comment: I like the option to do both but I think maybe the magnetic stirrer should have been the default and the propeller as the option.

 

6.  A new Wireless/ Wired 8.4 inch color touch panel controller (MCU).

MCU_screen_view_with_multiple_units

My comment: This only comes with the mid-range and the flagship models.  The controller can sit next to the titrator or be carried around like a clipboard.  Operators can control the titrator through protective glass if necessary.  I'm not sure how many people will elect to use the wireless vs. the wired connection but it's nice to have the added capability.  Nice.

7.  Multi-titrator integration.  The wireless/wired MCU can control up to 4 different titrators simultaneously (any combination of Karl Fischer or automatic titrator) 

MCU_controller for 710 series titrators

My comment: This feature is reserved for the flagship model.  I can see this being useful for those needing to run both moisture and acid for example.  Unfortunately the mid-level model MCU cannot be upgraded to the MCU flagship model so if you think you might expand later don't go with the S model.  Your better off getting the basic "B" model and then later tying them all together from the flagship model.

 710seriesmulticontrol

8.  Free method making software.

My comment:  All of the titrators now come with a CD that allows you to create methods on your PC and then transfer methods to the titrator.  You can also pull methods off of the titrator and edit it in the PC.  The software also comes with various popular methods pre-loaded to help get methods setup quicker.  I'm not so sure how robust this software is but free is nice.

CDstoredmethods
 
 
 
 




CONCLUSION:

Well I hope this was helpful in finding out quickly what the updates are for the new 710 series.  At this point since it's so new we will have to wait to evaluate how customers feel about their user experience and get their feedback on what they liked most and what they liked least.  If you have any questions or comments you can email me at info@scientificgear.com



 

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