Basis of Moisture Analysis Purpose The MA moisture analyzer can be used {for quick snd reisble determination ff the moisture content of materials of, iquid, pasty and solid substances using the thermogravimetrie method, Material When deductive methods are used, the “The moisture of a material is often ‘moisture content is determined indi- ristakeny equated to its water conten: rectly. A physical property related to the In fact, the moisture of 2 material rnoistre inthe substance is measured includes all ofthe volatile components (¢, absorption of electromagnetic ‘which are emitted when the sample +y3). These methods include Karl- is heated, imespective of the type of Fischer titration, infrared spectroscopy, material. Among such volatile substanc- rmierawave spectroscopy, ete Thermogravimetty is the process of water Getermining the Tass of mass that occurs fats hen a substance is heated. oils In this process, the sample is weighed sleohols before and after being heated, and the frganic solvent difference Between the two weights flavorings Setermined is calculated volatile components, products of decomposition (wen a sample ma conventional dying oven, is overheated) circulating hot air warms the sample {ram the outside inwards, Efficiency There are many methods for deter- 's lost during drying because as mining the moistre content of 3 sub- the moisture evaparates, it cools the stance, These methods ean be divided sample surface. into two categories: ‘By contrast, infrared rays OR rays) When absolute methods are used, the penetrate a sample without being moisture content is determined dineetly Impeded. Having reached the interior (or example, asa weight loss registered of 2 sample, they are converted into ddring the drying routine). These heat energy, ‘methods include oven drying, infrared drying and microwave drying, Al thre of these methods ate thermo= gravimetic, TRrays — alll Be OP GF ee20 A small percentage of IR rays reflected by the substance. The quantity of reflected IR rays depends to a great extent on whether the substance is ight oF datk in color. 2 ark substance light substance Jowreflecion high reflection How the rays penetrate the sample depends on the light-transmitting capacity of the sample. If the ght- transmitting capacity i Tow, rays can only penetrate the uppermost layers of the sample. The heat conduetivity ‘of the sample dictates the degree to Which the heat canbe transmitted to the underlying layers. The higher the conductivity, the faster and more tuniformly the substance is heated ‘The substance should be applied to the sample pan ina thin, even layer Aneight of approximately 2-5 mm for 5-15 g substance vcight has proved tobe ideal. Otherwise, the sample wal not be dried completely or the analysis time will be unnecessarily extended, 2 crust/skin will form on the surface of the sample or the sample will score, and the analysis results obtained vill not be reproducible (and therefore canvot be used), Pe Ke Incorrect application ofa sample When preparing substances for ‘measurement, do not use processes that generate heat, asthe heat generated may result in a loss of moisture prior to the measurement Perform initial analysis of a new substance to test how the I rays are absorbed by the sample and corverted into heat, A printout of the inter- ‘mediate values af the drying process provides you with this information at an early stage [Experience has shown that the tem= perature setting selected for infrared drying is usually lower than the temperature setting used when working with 9 drying oven. 1s many eases, the fully automatic shutoff mode will meet your requite- iments. 1 the final result is higher or Tower than expected, ty varying the temperature setting before resorting toa different shutoff parameter ‘When analyzing the samples that lose {heir moisture only very slowly oF when ‘operating a cold moisture analyzer the fully automatic mode may end the dying routine ton early sitee no ana Iyzable progress inthe drying routine «ean be detected, In this case, preheat the moisture analyzer for 2-3 minutes before starting the drying routine, or select a different shutoff parameter. ‘The Sartorius Moisture Analyzer Applications Guide provides you with important information on the wse of ‘your moisture analyzer.Preparation ‘Make sure you cany out the following preparations prior to drying a sample = Adjustment to the available measuring system (ifrequited) ~ Sample preparation = Setting the drying program parameters Adjustment to an Existing Measuring System ‘A moisture analysis method often replaces another drying method (such as oven frying method) because it simple fo se and requires shorter analysis time In this case, you should adapt this method to that of the moisture analyzer in order ‘to obtain values comparable to those yielded by your standard reference method Perform parallel measurements: take a fresh sample and divide i in half Determine the moisture content of the first haf using your standard method of analysis Analyze the second half of the sample in the moisture analyzer. Use the following settings: = fully automatic mode forthe shutoff parameter ~ Tower temperature settings than for the oven drying method = temperature setting for organie substances: 80 100°C = temperatie setting for morganic substances: 140=160°C I the result ofthe second analysis does not comespond to that ofthe fist = repeat the analysis first using a different temperature setting = then vse the semi-automatie mode for the shutoff parameter (for example with 2 ciferent Toss rale pr 24 5) ‘Vary the shutoff parameter if requited = Increase end-point recognition: set the parameter to 2 mgl24 s or 1 mgl24 s = Decrease end-point recognition: se the parameter (o 10 mgl24 s oF 20 mg/24 s a2 Sample Preparation Selecting a Sample © Select a representative part of the whole substance as a sample ~ a representative numberof individual sarapes For quality control = Samples which indicate a trend are sufficient for in-process control required, homogenize the product before a sample is taken by = mixing or sting, ~ taking several samples from different ateas of the produ, oF taking several samples at defined intenals (© Toke only one sample ata time fora given analysis and prepare it a quickly as possible “This way it wll ot lose or gain moisture asa result of the ambient conditions. I.you need to take several samples simultaneously, the samples must be sealed in air Light containers co ensure that the storage conditions do not alter the state or condition of the samples = Warm or highly volatile substances lose their moisture very quickly. = Storing samples in 3 container may Tead {o moisture condensing on the walls of the container =f the container is too Targe, moisture is passed to the at remaining in the container © Mix the condensed moisture back in with a sample, if necessay. Preparing a sample (© When crushing a sample, avoid any contact with heat Heat results in moisture loss. (© Crash a sample with = apestle =a shredder (ee below) For liquids containing solids, use = glass stiner =a spoon, or = a magnetic ste. Use an appropriately designed tool for shredding a sample, ‘Using disposable sample pans © Use only Sartorius disposable sample pans (inner diameter of 82 mm. Reusing sample pans leads to poor reproducibility of results for several reasons: ~ sample residues can yemain on the pan even after cleaning ~ residues from cleaning agents can evaporate during the next moisture analysis ~ seratehes and groaves made during leaning result in damage that forms points of attack for hot, rising air produced during the drying process {more pronounced buoy- ang)ng a Sample to the Sample Pan © Apply the sample tothe sample pan in thin, even layer (height: 2 to 5 mm, weight: 5 £015 g); otherwise: = a sample applied unevenly will result in @ non-uniform distitbution of heat = sample will not be dried completely ~ the analysis time will be prolonged unnecessarily = the sample bums or a crust skin forms om its surface asa result of a very thiek layer ~ the crust makes it difficult or impossible for moisture to escape from the sample during the drying process = an uncertain and unknown quantity of mofsture remains in the sample XX © Apply quid samples, pasty samples or samples that an melt to a glass fiber filter (order no, 6906940}; advantages include: = wniform distribution due to capillany effect ~liguids prevented from beading together and forming drops = moisture can evaporate faster with larger surfaces = considerably more convenient than the "sea-sand method” When drying samples containing sugar, a erast or skin can form and seal the surface. A glass fiber filter is particularly useful in such cases. The moisture cn evaporate downwards through the surface ofthe filter. You ean prevent of limit erast/skin formation by placing the glass fiber filter on top ofthe sample © Cover solid, heat-sensitive samples with a glass fiber filter (order no. 6806940); advantages include: = gentle heating; sample surface is shielded from excessive heat higher temperature setting ean be selected = uniformity of the sample surface faster evaporation of the moisture ~ excellent reproducibility for samples containing fat Preventing the formation of erust/skin Solvents can be applied to the sample to prevent the formation of erust/skin during anl- ysis. The solvent applied has no bearing on the final result of an analysis {© Re-open the sample chamber within 2 seconds of closing i after the beep tone). © Apply a solvent to the sample {© Close the sample chamber and start the analysis as usual a2 Operating the Moisture Analyzer Setting the Drying Parameters Purpose the moisture analyzer to the special requirements of products. Parameters can be configured individually for each program, Drying Parameters (Overview) Factory set Program memory (erocrary + Program name L teating program —-o stanaby ° temperature Cc F tnt weight ——- 0 start of analysis L End of analysis [Display mode L print ° intermediate result } Determination of —-o ignition residue, fess > 1 Factory settings —- oo Blank (max. 16 characters) Standard drying Temperature Gentle drying TT Temperature Time on (On ——— Temperature ow O) ——— Target With stability when Enter pressed Without stability When cover is elosed With stability When cover losed Fully automatic Semi-automatic Loss Absolute Time interval Semi-attamatie Loss Percentage Time interval Time Crime Manual Moisture (1) Dry weight (R) Ratio (LR) Weightloss (mg) Residue (g) Residue weight (g/kg) Gramflite (gf) Sample ow 0 ——— interval on on Line 1 Line 2 No Yes gd es tose 105¢ 3.0 min, aore 50g 5mg 2s 1% 60s. 150 min ot min mpty Empty 40 .. 220°C for MA1500, otherwise 40... 180°C 40 .. 200°C for MA1500, otherwise 40... 180°C 1,0. 20 minvtes 40... 100°C 0.2 g... 90% max load 1..50mg 5. 3008 01. 5.0% 5. 200 0.1. 99.9 minutes 0.0001 .. 9.99991 0,1. 10.0 minutes max. 20 characters ‘max. 20 charactersFeatures Number of Drying Programs 20 programs Programs are listed according to program number. Heating Programs Two heating programs are available for performing moisture analysis of a substance: Standard drying Gentle dying Standard drying: The final temperature needs to be centered when using the standard program, Teo) al Ia target temperature of over 200°C is entered, the moisture analyzer heats to the target and then adjusts to 200°C in 5 phases, from the 10° to the 30 minute 10 30 [min] Gentle drying eat up to the target temperature (maximum 200°C) ina selectable time frame between | and 20 minutes, Standby Temperature ‘Temperature set to defined value ‘when the sample chamber is closed Initial Weight ‘The target weight (as a guide for applying a sample to the analyzer ~ potas 2 starting condition) can be entered by the user. The tolerance Timits of # 20% are displayed. Start of Analys stability after pressing ia) key: When START is shown jn the Function Fine and you press Ge) to confimn, the intial weight is stored at stability regardless of whether the cover is pen or closed Without stability after the cover is dosed A prompt to close the cover {a graphic symbo} is displayed once {he intial weight condition is met. ‘The inital weight is stored without stability as soon as the sample chamber is closed ‘The anabsis stars as soon as a 2-second delay has elapsed after the cover is closed or the sample chamber is opened and then closed {applies to both start. criteria) With stability after cover is closed A prompt to close the caver (a graphic ‘symbol is displayed once the initial ‘weight condition ism he initial weight after stability is stored 25 soon as the sample chamber is closed, There is no adéitional delay time Intemuption of analysis: You can open and close the cover at any time without interrupting the ‘measurement to post-treat samples ‘The device status lie shows ‘MEASUREMENT PAUSE/MEASURE- ‘MENT when you openjelose the cover The drying and heating algorithms stop ‘when the cover is open and continue ‘once it closed End of Analysis with Shutoff Parameters Folly automatic Semi-automatic, absolute Semi-automatic, percentage Timer mode Manual Fully automatic: The analysis ends 4s soon as the weight loss per 24 s below an automatically detected threshold, eight Moisture Tine Semi-automatic, absolute: ‘The analysis ends as soon as the weight loss per 24 sis lower than a user= defined threshold (stim miligrams), Semi-automatic, percentage: ‘The analysis ends as soon as the weight loss per 24 sis lower than a user= defined threshold (set percent). The percentage is entered by the user Timer mode: The analysis ends as soon asthe specified time has elapsed, Manual ‘Shut-off with the Ge) Key.Display Mode The following units can be selected for displaying analysis results = Moisine = Dry weight = Ratio = Weight loss = Residual weight ~ Residual weight = Gramflter . wR IR mg @ sh sf Print Intermediate Results = When set to “Of”, intermediate results ean only be printed by pressing the CAD key, = Intermediate res can be printed out automaticaly after» configurable time interval Determination of Ignition Residue A two-part measurement ean be performed using this setting. Example: ‘Moisture analysis and incineration of sludge, Moisture content is analyzed inthe fist stage, The sample s then ‘reduced to ashes inthe fumace and inthe second stage the ash is caleulated 38 a percentage of the initial weight CONTINUE is displayed instead of END after the frst stage. The moisture analyzer must not be used for other purposes between the fist and second stages. Headers Text can be entered forthe drying ‘report (2 Hines each with max. 20 characters) The relevant line is hot printed ifn text is entered Factory Setting ‘The drying programs can be reset to the factory settings 26 Printout of the Analysis Parameters When the desited program is displayed Press the C2 key Printout (example on right). Lines with ‘more than 20 characters ate truncated. Additional Functions ‘The following funetions are supported fn the program memory: Display programs Change settings Save program changes 14.07.2006 12:40 Model MA150a-000230V Ser. no. 18701636 Vers. no. 01-50-01 1D PROGRAM Pt Program name Progr. name: MEYER Heating program Standard drying Temperature 105 °c Standby temperature oft Initial weight oft Start of measuremen Without stability, after close End of measurement Fully automatic Result display Moisture cay Print intermediate ort Determination of ignition residue off Headers Line 1 Line 1: Line 2 Line 2:Example: Standard Drying with Fully Automatic Shutoff Mode The moisture content of 2 g of com starch isto be analyzed. The sample ean scorch The analysis isto be ended automatically as soon aa constant weight is reached. Settings (changes inthe factory settings) Program number: 1 Final temperature: 130°C Start of analysis: With stability after Enter ey is pressed End of analysis: Fully automatic (factory setting) Part A: Configuring drying parameters f overheated but isnot particularly heat sensitive se erin sete ns 2 select Potan econ Deo FER + O0929 = sews insim “Tane — - — a ii 2step Key for instruction) Display/Printout 8. Confirm temperature value 9. Sclect the Bar graph For weighing-in sample parameter 10 Confirm far oraph For weighing-in sample parameter 11, Select the On setting and confirm 12, Enter the target weight 2.8 13. Confirm the target weight 14, Select the Start analysis parameter Confirm the Start analysis 16, Select the with stab after ENTER key setting and confinn 17, But the PROGRAM Function 28Part B: Performing the analysis Step Key (or instruction) Display/Printout 1, Tum on the moisture analyzer 2, Prepare the sample: Nol necessary with corn starch 3. Open sample chamber and position a new sample pan 4, Tare the sample pan: Select the TARE function and confirm 5, Distibute approx. 2g of com starch evenly om the sample pan 6. Start the drying program The analysis report header is printed after adelay of 2 seconds (printout: see next page) we CD or PD as needed \ Close sample chamber Sartorius logo is displayed Selftest rans Tse aaa, + dc204dbe + O092¢9 = SETUP. PROGRAM “Does ac 4 SDS6S ee XE TTSeC Auta, + eD4bs XE 2step Key for instruction) 20 The current moisture loss is then displayed Foully-automatie shut-off of the drying process once no more loss detectable (after 5.2 minutes in this case) Then the footer ofthe analysis report is printed out Display/Printout 14.07.2006 1 ? Model MA150a-000230V OOS wt. ig a tem. STM SONe stay temps, ore ive «200885 ae 2 + ID90” Szain END ee