Operation Manual for - Mrclab.com

Ultrasonic milk analyzerSwitching Adapter• Input:100 - 240 V ~1.6 A max.50-60 Hz• Output: +12 V 4.17А min.• Output power:50 - 65 WMeasurement modes• cow milk• sheep milk• UHT milk• goat milk• buffalo milk• cream• whey• recovered milk• other /pasteurized milk/CAUTION!Keep the switching adapter dry!Please, read and follow strictly all the instructions in the manual.Due to continuous improvement in the device, information contained in thismanual is subject to change without notice. Contact the company-producerfor revisions and correctionsOperation manual 2/98

Ultrasonic milk analyzerSAFETY INSTRUCTIONS1. Read this manual carefully and make sure that you understand all theinstructions.2. For safety purposes the device is equipped with grounded powercable. If there is no grounded electrical outlet where the device willbe used, please, install such before using the device.3. Place the device on leveled and stable plate. In case it falls or isseverely shocked it may be damaged.4. Connect to the electrical network in such a way that the power cableto stay away from the side for accessing the device and not to bestepped on.5. Every time before cleaning the device switch it off and unplug it fromthe electrical outlet. The device has to remain unplugged till thecleaning completion.6. Do not disassemble the unit in order to avoid possible electricalshock. In case of malfunction contact your local dealer.7. Handle the liquids the device works with carefully, following all theinstructions for their preparation.8. Place the switching adaptor in such a way as to be protected fromoverflow and spillage of liquids.Operation manual 3/98

Ultrasonic milk analyzerPARTS AND ACCESSORIESIn the table below the standard delivery configuration of the milk analyzer islisted:№ Description Item № pcs1. Ultrasonic portable milk analyzer LSS001 190 sec.1 sample measurement time60 sec30 sec2. Operation manual LSS002 13. Plastic sample holder LSS003 24. Spare Pipes LSS004 25. 12 V DC Power Supply Cable LSS005 16. Alkaline cleaning solution Lactodaily 100 g 17. Acidic cleaning solution Lactoweekly 100 g 1In the table below the milk analyzer spares and accessories, which aredelivered on customers request are listed:№ Descriptiona) included in the set:b) not included in the set (may beadditionally bought):Item №pcs/8. RS232 Interface Cable - Analyser-IBM PC LSS0069. Service Pack - CD LSS00710. Handle LSS008 111. pH measuring system LSS009 112. pH probe with cable and holder LSS010 113. Buffer solution Ph 60 ml LSS011 1(pH7.00±0.01/20˚C)14. Buffer solution pH 60 ml LSS012 1(pH4.00±0.01/20˚C)15. Milk conductivity measuring system LSS013 116. Buffer solution conductivity 50 ml (5.02 LSS014 1(±5%) mS/cm (18±0.1˚C)17. Real time clock LSS015 1Operation manual 4/98

Ultrasonic milk analyzer18. ECS POS Serial Printer LSS017 119. 12 V Serial Printer Power Supply Cable LSS018 120. RS232 Interface Cable - Milk Analyser – LSS019 1Serial Printer21. Carrying case – plastic LSS020 122 Plug type11Operation manual 5/98

Ultrasonic milk analyzer1. FUNCTIONThe function of the milk analyzer is to make quick analyses of milk onfat (FAT), non-fat solids (SNF), proteins, lactose and water contentpercentages, temperature ( o С), pH, freezing point, salts, conductivity aswell as density of one and the same sample directly after milking, atcollecting and during processing.Operation manual 6/98

Ultrasonic milk analyzer2. TECHNICAL PARAMETERS2.1. Working modes characteristics:The program of the milk analyzer has four working modes.2.1.1. Measurement mode milk / dairy product – first type2.1.2. Measurement mode milk / dairy product – second type2.1.3. Measurement mode milk / dairy product – third typeThese modes have been calibrated on customers’ request for 3 milk typesfrom the following: cow, sheep, UHT, buffalo, goat, camel milk, cream, icecream mixtures, whey, recovered milk, etc. before leaving the productionfacilities and the text on the display will be for the corresponding types, as isindicated on page 2 Measurement modes.2.1.4. CleaningOperation manual 7/98

Ultrasonic milk analyzer2.2. Measuring range:Fat ………………..................... …………………...from 0.01% to 25%SNF ……………………………… ...…………………....from 3% to 15%Density * ………………………. ……...…….from 1000 to 1160 kg/m 3Proteins …………………………. ………………………..from 2% to 7%Lactose ………………………... …………………..from 0.01 % to 6 %Water content ………………… ……………...……..from 0 % to 70 %Temperature of milk …………… ……………………..from 1 o C to 40 o CFreezing point ………………… …………..from – 0,400 to – 0,700 o CSalts ……………………………. ……………...………from 0,4 to 1,5%PH** ……………………………... …………………..………from 0 to 14Conductivity** ………………… ……………...…from 3 to 14 [mS/cm]* Density data are shown in an abbreviated form. For example 27.3 have tobe understood as 1027.3 kg/m 3 . To determine the milk density, write downthe result from the display and add 1000.Example: result 21,20; density = 1000 + 31,20 = 1031,2 kg/m 3** pH and conductivity measurements are optional and are delivered oncustomers' request.The abbreviated form of the density is used also when entering data forsamples in working mode Recalibrate, for example:If the measured sample density is 1034.5 kg/m3, then in the menu forentering the samples parameters used for calibration, across the parameterDen = , you have to enter 34.5.2.3. Maximum permissible absolute error:Fat …..……………………………….. …...………………….…….± 0.1%SNF ………………………………….. …………...………….…...± 0.15%Density ……………………………… ………………………..± 0.3 kg/m 3Proteins ……………………………... ……...……………….…...± 0.15%Lactose ……………………………… .………………………….....± 0.2%Water content ………………………. .…………………………….± 3.0%Temperature of milk ……………….. .………………………………± 1 o CFreezing point……………………….. ..……...…………………± 0.001 o CSalts ………………………………... …..…………...…………...± 0.05%PH** …………………………………. ……………………………±0.05%Conductivity** ………………………. ……………………………...±0.05The difference between two consequent measurements of one and the samemilk could not exceed the maximum permissible absolute error.Operation manual 8/98

Ultrasonic milk analyzer2.4 Correct ambient conditions:Maximum permissible absolute error is guaranteed in case of normal ambientconditions:Air temperature………………………… ….………….from 10 o C to 40 o CRelative humidity ……………………… ……………...from 30% to 80%Power supply ………………………… …………………...220V (110V)extent of contamination at normal environmental conditions…………..2Maximum permissible absolute error values in point 2.3 are in dependenceon the correctness of the corresponding chemical method, used forcomponent content determination. In point 2.3. are used the followingreference methods: Gerber – for fat, gravimetric – for SNF, Kjeldahl – forprotein. The boundary for maximum variation of repeatability when the powersupply voltage is from +10 to – 15% from the nominal voltage values (220 V)have to be no more than 0.8 accuracy according point 2.3. The analyzer isused in conditions free of outer electrical and magnetic fields (except themagnetic field of the Earth) and vibrations.2.5. Dimensions:………………………….240/220/100 mm, mass 3,0 kg2.6. Continuous working time:…….…….………………………….…...……....non-stop2.7 Milk sample volume per one measurement:………………………………..………..25 cm 3(= 25 ml)Operation manual 9/98

Ultrasonic milk analyzerfig. 2 Back panel1. Holder for pH-probe ∅12 (option) 6. Serial interface RS2322. pH-probe (option) 7. 12 V printer output3.Handle (option)8. 12 V input4. pH-meter input (option) 9. Power switch5. Serial printer interface 10. Switching adapterOperation manual 11/98

Ultrasonic milk analyzerFig. 3 Principle working schemeOperation manual 12/98

Ultrasonic milk analyzerFig. 4Peripherals connectionOperation manual 13/98

Ultrasonic milk analyzerFig. 5Cable Description90-1801-0008RS232 Interface Cable - Milk Analyser – Serial Printer90-1801-0010RS232 Interface Cable - Milk Analyser – IBM PC2. TxD3. RxD5. GNDMilkAnalyserDB 9-pinmalePCDB 9-pinfemale2. Receive Data(RxD)3. Transmit Data(TxD)5. Signal Ground(GND)90-2001-0001Probe pH with cable90-1801-0009DC 12V Power Supply Milk Analyzer Cable1. GND2. No connection3. No connection4. 12V DCOperation manual 14/98

Ultrasonic milk analyzer3. QUALIFICATION OF RAW MILK, THERMALLY TREATEDMILK, OTHER DAIRY PRODUCTS AND DERIVATIVES3.1. Taking samples and preparation for analysesIn order to receive reliable results in qualification of milk, dairy products andderivatives are needed: precise samples taking; correct samples storing (inneed to be preserved); correct preparation before making measurement. Therules and requirements for this are described in details in Appendix PreparingSamples.3.2. Making the measurement.3.2.1. Preparing the analyzer for working mode3.2.1.1. Put the analyzer on the working place, providing good ventilation andnot in the vicinity of heat providing devices or sources. The temperature in thepremises has to be in the boundaries 10-30 o C.3.2.1.2. Check if the power switch is in "0" position and that the outlet voltagecomplies with the voltage indicated on the rating plate of the analyzer.Connect the power supply cable to the electrical outlet.3.2.1.3. Switch on the “POWER” button, which starts the identificationprocedure. For a short time the display shows the number of the softwareversions, for example:where:Milkanalyzer xxxLCD vers xxMA vers yyMA ser. N. xxxxMilkanalyzer xxx is the time for measurement.LCD vers XX is display control software version.MA vers YY is the motherboard software version.MA ser. N. xxxx is the serial number – written on the rear panel of theanalyzer.These data are called analyzer’s IdentityOperation manual 15/98

Ultrasonic milk analyzerIf in the process of exploitation there is a need to ask a question thecompany-producer, you have to send the data, written on the display duringthe above described initialization procedure i.e the analyzer’s identity.3.2.1.4.Till the analyzer is prepared for work (at about 5 minutes) thefollowing message is written on the display: “Getting ready”. Above pointedtime is in dependence of the environmental temperature and increases withdecreasing the temperature.3.2.1.5. When the device is ready for work the display shows: “Ready tostart”.The analyzer is ready to make analyses in mode 1 (normally Cow)3.2.1.6. If you want to pass to another mode press the button Enter and holdit pressed. The following message appears on the display:Release button tostart menuRelease the button Enter. The display shows the possible working modes:Milk selectorCal1 – CowCal2 – SheepCal3 – UHT------------------------------CleaningUsing “up”▲and ”down”▼buttons, choose the working mode and press Enterin order to start it.3.2.2. Making analysesTo start measurement: pour the preliminary prepared sample in the sampleholder of the analyzer; put the sample holder in the recess of the analyzer;press the button Enter.Operation manual 16/98

Ultrasonic milk analyzerThe analyzer sucks the milk, makes the measurement and returns the milk inthe sample-holder. During the measurement the temperature of the sample isshown on the display.Ignore the results received immediately after switching on the analyzer andafter measuring distilled water. Make a second measurement with newportion of the same sample.3.2.3. Displaying the results3.2.3.1. When the measurement is finished, the sample returns in thesample-holder and the display shows the results. For example:Where:Results:F=ff.ff S=ss.ssD=dd.dd P=pp.ppL=ll.ll W=ww.wwF= ff.ff - measured FAT in percentage;S= ss.ss - measured SNF in percentage;D= dd.dd - measured density in percentage;P= pp.pp - measured protein in percentage;L= ll.ll - measured lactose in percentage;W= ww.ww - measured sample’s added water in percentage.By pressing the button” Down” ▼ the display shows the second page,containing the results:Page 2 Results:T=tt.tC pH=pp.ppFP=-0.fff sol=0.sssWhere:tt.tCpp.pp-0.fff0.sss- sample’s temperature;- sample’s pH result – if there is a pH probe connected;- measured sample’s freezing point;- measured salts values;Operation manual 17/98

Ultrasonic milk analyzerBy pressing the buttons “up”▲ and ”down”▼, the operator has the possibilityto pass from one page result to another.If the device has an embedded option “Conductivity” and "conductivitymeasurement" started, the result is shown on the display, showing the basicresults replacing lactose results in the following way:C=xx.xxIn this case the Lactose result is shown on a new page - Page 3 Results.xx.xx is the measured milk sample’s conductivity in [mS/cm]. If the results areoutside the limits for this type of sample (see table from the AppendixConductivity measurement), the cursor flashes after the letter С, remindingthat the sample is not correct. On the printout it is printed as !!!.If the conductiity value is outside measuring range (2-14 mS/cm), thefollowing message appears on the display:C=OutRg (Out of Range), and on the printout there isn’t any line withconductivity value.3.2.3.2. Write down the results in the form. The results remain on the displaytill a new measurement is started. If the analyzer is connected to a computeror a printer, it sends the data to the computer or prints them.Operation manual 18/98

Ultrasonic milk analyzer4. CLEANING THE ANALYZERThis procedure prevents gathering milk fat residues and milk stone on thesensor. The milk stone consists of milk solids, calcium, iron, sulphates,magnesium, etc. All these substances form layer on the pipe and sensor’swalls, which leads to deviations in the measurement results and blocking upthe piping.The company-producer recommends usage of the chemicals, supplied withthe analyser – alkaline and acidic (Lactodaily and Lactoweekly). You mayorder them separately or together with the analyser. Try to use only thesechemicals for cleaning the analyser.Do not use chemicals not intended for usage in the milking systems orvessels in the dairy sector. Pay special attention to the concentration of theacidic chemical. Increased concentration may damage the measuringsensor.4.1. Periodically cleaning (rinsing) the analyzerIt is done in the process of routine work of the analyzer. Its aim is to preventdrying up and adhesion of different milk components in the milk analyzer’smeasuring system.4.1.1. Periodical cleaning frequency.It is easy to understand what is the period on which the rinsing could be doneas the analyzer reminds you when it is necessary. This is done by a soundsignal in 1-second cycle after the set time intervals elapse:• 55 min. after switching on the power supply of the analyser, but idlework;Operation manual 19/98

Ultrasonic milk analyzer• 15 min. after the last measurement of real milk sample.After cleaning completion, new measurement takes place in above describedtime intervals.The following message appears on the display:Time to startcleaning4.1.2. Making the rinsingAfter above message is received put in the recess of the analyzer a sampleholder with alkaline cleaning solution or water.Press Enter to start the rinsing mode.In this mode the analyzer makes 8 cycles and stops.Already used solution is poured out of the analyser. Now the device is ready forthe next measurement. In case of doubt that the analyzer is still not wellcleaned, the procedure Cleaning may be executed repeatedly.4.2. Complete cleaning4.2.1. Complete cleaning frequencyThis cleaning is done after finishing the work with the analyzer at the end ofthe working day or if it is obvious that the measuring system of the analyzer iscontaminated in case of intensive work with it. It is done with alkaline cleaningsolution.Preparation of 1 % alkaline solution of Lactodaily for circulation cleaning inthe milk analyzer:1. Take the package 100 g concentrated powder chemical Lactodaily2. Carefully cut the upper end, paying attention not to spill it.3. In appropriate vessel (for example bucket) pour 1 l water.4. Add the powder and then again water up to 10 l.Then follow the instruction for milk analyzer cleaning.4.2.2. Cleaning4.2.2.1.Rinsing milk residuesFill in the glass with water. Put it in the recess of the analyser and startcommand Cleaning from the main menu. After finishing it pour out thecontaminated water.4.2.2.2.Cleaning with alkaline cleaning solutionOperation manual 20/98

Ultrasonic milk analyzerFill in the glass with warm (50-60 С) alkaline cleaning solution. Put it in therecess of the analyser and start the command Cleaning from the main menu.After finishing it, pour out the contaminated liquid.4.2.2.3.Rinsing with waterFill in the glass with water. Put it in the recess of the analyser and startcommand Cleaning from the main menu. After finishing it pour out thecontaminated water. Now the device is ready for work.4.2.2.4. Cleaning with acidic solutionIt is recommended to be done every day.Preparation of 1 % acidic solution of Lactoweekly for circulation cleaning inthe milk analyzer:1. Take the package 100 g concentrated powder chemical Lactodaily2. Carefully cut the upper end, paying attention not to spill it.3. In appropriate vessel (for example bucket) pour 1 l water.4. Add the powder and then again water up to 10 l.Fig. 6 Labels for the cleaning chemicalsThe following procedure is executed:1. Rinsing the milk residues:Fill in the glass with water. Put it in the recess of the analyser and startcommand Cleaning from the main menu. After finishing it pour out thecontaminated water.2. Cleaning with acidic solutionFill in the glass with warm (50-60 С) acidic cleaning solution. Put it in therecess of the analyser and start the command Cleaning from the main menu.After finishing it, pour out the contaminated liquid.3. Rinsing with waterFill in the glass with water. Put it in the recess of the analyser and startcommand Cleaning from the main menu. After finishing it pour out thecontaminated water. Now the device is ready for work.Operation manual 21/98

Ultrasonic milk analyzerIMPORTANTTHE MAIN REASON FOR MALFUNCTIONING OF THEDEVICE IS THE BAD CLEANING OF THE SYSTEM AFTERMAKING ANALYSIS.In case of malfunction due to the bad cleaning of theanalyser your guarantee is not valid anymore and anyrepair has to be paid.4.3. Peristaltic pump serviceFig.7 Peristaltic pumpOperation manual 22/98

Ultrasonic milk analyzer5. POSSIBLE MALFUNCTIONS AND ERROR MESSAGES,TROUBLESHOOTINGIn the table below are described the possible malfunctions during the milkanalyzer’s exploitation and ways for their repair/remedy. If the problempersists after all recommended measures are taken, please, connect thenearest service center for help. Do not forget to tell the analyser’s identity.To receive the analyzer’s identity, refer to point 3.2.1.3.ErrormessageMAoverheatedAccompaniedby acontinuoussound signalEmptyCameraPossibleproblem/causeOverheatedmilkanalyzerInsufficientquantity ofthe milksamplesucked inthe systemor air in thesampleRepair/remedyImmediately switch off the analyzer.Pay attention the analyzer to be situatedaway from direct sunlight or heating devices.Wait 5-10 minutes the device to cool down orto be normalized the ambient temperatureand switch it on again.The analyzer is ready to measure the nextsample. In order to avoid the futureappearance of the same error message,please, check the following:- The sample is prepared according theinstructions and there aren’t air bubblesin it.- There is a real suction of the sampleafter starting measurement, i.e. it isobvious that the level of the milk samplein the sample holder decreases. In othercase – there is damage in the suctionsystem.- Avoid the end of the suction pipe to beabove the surface of the liquid (notdipped enough).- Avoid curdling of the milk sample. Cleanimmediately if there is a sample curdledin the system.- In mode Measurement, after starting themeasurement, remove the sampleholder and see if there is no milk pouredOperation manual 23/98

Ultrasonic milk analyzerSampleOverheatSuckedoverheatedsampleback in the sample holder.The analyzer is ready to measure the nextsample. In order to avoid the futureappearance of the same error message,please, check the following:-The sample is prepared according theinstructions and its temperature does notexceed the maximum permissible sample’stemperature.-Complete the procedure for checking theanalyzer in case of error message EmptyCamera.Operation manual

Ultrasonic milk analyzer6. MAKING CORRECTIONS AND RECALLIBRATION OF THEDEVICEIn the process of work with the analyser there is a possibility the results tostart differing between the data for some of the measuring parameters whenmeasured with the milk analyzer and the corresponding reference method ofanalyses (Gerber for fat, Kjeldhal for proteins etc). In order to establish thepossible discrepancy and to correct the readings of the milk analyser do thefollowing:6.1. Taking samples and preparation of samples for checking theaccurracy of the milk analyser, making corrections andrecalibrationThis is a basic moment for the correct checking the accuracy of the analyserand for making correct and precise correction and calibration. It isaccomplished according Appendix Sampling and preparation of samples forverification the accuracy of the milk analyzer, making corrections andrecalibration.6.2. Determination the type of the discrepancy:6.2.1. Making measurementsMake measurements with different samples (not less than 3) with knownvalues of a separate parameter (for example fat content), determined by theknown reference methods of analyses (for example Gerber's method fordetermination of fat content). For more accuracy it is recommended amongthese samples to be also such with values, close to the lowest and highestbounds for the measured parameters.Make 5-time measurement for each of the samples. Calculate the averagevalue for each sample parameter, without taking into consideration the firstmeasurement for each sample.6.2.2. Analysing the measurement resultsMake comparison between the values of the parameter from the referencesample and measured with the analyser. Make analyses of the differencereceived.6.2.2.1. If the received differences are relatively constant value for sampleswith different content of the analysed parameter, it is necessary to makecorrection.Operation manual 25/98

Ultrasonic milk analyzerFor exampleМ% of the reference samples: 2,20 3,00 3,80 4,60 5,20М%average when measuringwith the analyser: 2,38 3,17 4,01 4,79 5,42Difference: 0,18 0,17 0,21 0,19 0,22Conclusion: the difference is relatively constant value and correction ispossible to be done with – 0,2 % (see Corrections, p6.3.3)6.2.2.2. If the differences are not a constant value it is necessary recalibrationto be done.For example.М% of the reference samples: 2,20 3,00 3,80 4,60 5,20М% when measured with theanalyser: 2,02 2,93 3,76 4,75 5,44Difference: -0,18 -0,07 -0,04 0,15 0,24Conclusion: It is obvious that the difference is variable value andrecalibration have to be done (See Recalibration, p.6.4).6.3. Making corrections6.3.1. Possible corrections, limits and changing stepsEvery parameter from each calibration may be separately corrected. Below isthe table with possible corrections, limits and changing steps:Parameter Increasing Decreasing StepFAT 0.95% 0.95% 0.01%SNF 4.75% 4.75% 0.05%Density 4.75% 4.75% 0.05%Lactose 0.95% 0.95% 0.01%Salts 0.95% 0.95% 0.01%Proteins 0.95% 0.95% 0.01%Added water 9.00% 9.00% 1.00%Sample’s temperature 9.90 o С 9.90 o С 0.1 o СOperation manual 26/98

Ultrasonic milk analyzer6.3.2. Preparing the analyzer for mode Corrections6.3.2.1. Press the button Enter and without releasing it switch on the powersupply of the device, wait for the starting identification messages and releasethe button after the following message appears on the display:Release buttonto start setupAfter releasing the button on the display is shown:MA Setupfollowed by possible to be entered by the operator menus:Special modesCorrectionsSettings------------------------------TestspH & Co MeterExit6.3.2.2. By using buttons “up” ▲ and “down” ▼position on Corrections andpress Enter.6.3.3. Making correction6.3.3.1 Determining the correction modeWhen starting Corrections, the following appears on the displayCorrections:Calibration 1Calibration 2Calibration 3---------------------------TemperatureExitOperation manual 27/98

Ultrasonic milk analyzerBy using buttons “up”▲ and ”down”▼position on the correspondingcalibration (for example Correction 1 – cow) and press Enter.6.3.3.2. Choosing correction parameterAfter choosing calibration mode the display shows the following:Cal1 Correct’sFATSNFDensity------------------------------LactoseSaltsProteinsWater------------------------------ExitUsing the buttons “up”▲ and ”down”▼position on the parameter to becorrected (for example FAT) and press the button Enter.6.3.3.3.Making correctionAfter choosing parameter (for example fat) the display shows the following:FAT Correction0,05- OK +Using the buttons “up”▲ and ”down”▼is possible to increase or decrease thevalue of the measured parameter in the above pointed limits. Leaving thismode means saving the correction value and activating it.6.3.3.4. Making verificationAfter the corrections are made put the milk analyser in working modefollowing the sequence below:1. Switch off the power supply.2. Switch on the “POWER” switch which starts the identification procedureFor a short time the display shows software versions of the analyzer, forexample:Operation manual 28/98

Ultrasonic milk analyzerMilkanalyzer xxxLCD vers xxMA vers yyMA ser. N. xxxxWhile the abalyser is ready for work, the display shows “Gettingready”3. After the analyzer is ready for work a sound signal is heard and thedisplay shows: “Analyzer ready”. Now the analyzer is ready for makingmeasurement in the first measuring mode (most often Cow).4. make measurement of reference samples with known values of thecorrected parameter several times. If the difference between the valuesof the parameter from the reference methods and milkanalyser are inthe limits for the parameter it may be considered that the correction issuccessfully made.If the discrepancy between the measurements from the milk analyser andclassical methods is bigger than is necessary to make second correctionaccording above described way.If after the second correction the results are unsatisfactory we recommendmaking a calibration of the analyser. In dependence of the conditions andyour requirements you may make the calibration using a personal computertype IBM PC and the company's calibration program or autonomous - byrecalibration.When making corrections or calibrations be 100% sure in the accuracy of thereference methods result.6.4. Recalibrating the milk analyser6.4.1. Running the analyser in mode Recalibrate6.4.1.1. Press the button Enter and without releasing it switch on the powersupply of the device, wait for the starting identification messages and releasethe button after the following message appears on the display:Release buttonto start setupOperation manual 29/98

Ultrasonic milk analyzerAfter releasing the button on the display is shown:MA SetupFollowed by the possible to be entered by the operator menus:Special modesCorrectionsSettings------------------------------TestspH & Co MeterExit6.4.1.2. By using buttons “up” ▲ and “down” ▼ position on Settings andpress button Enter.6.4.1.3. Analogically, position on Recalibrate and press the button Enter.6.4.2. Making recalibration6.4.2.1. Determining the calibration modeAfter starting Recalibrate, the display shows the following:RecalibrateCalibration 1Calibration 2Calibration 3-----------------------------Edit samp’s 1Edit samp’s 2Edit samp’s 3Edit FrPoints-----------------------------ExitUsing the buttons “up” ▲ and “down” ▼ position on the correspondingcalibration (for example if you need to recalibrate cow milk, which is assignedin the milk analyser as Calibration 1 - cow) and press the button Enter.Thefollowing message appears on the display:Operation manual 30/98

Ultrasonic milk analyzerCalibration 1Getting ready6.4.2.2. Entering values for the separate sample parametersWait for the sound signal and the following menu on the display:Cal1 Samp HighFat=f.ffSNF=y.yyDen=d.dd------------------------------Lac=l.llSol=s.ssPro=p.ppExitIn this display is possible to be entered the results from the milk with highFAT chemical analyses, which were received by the methods from AppendixMethods.For example:- by using the buttons “up” ▲ and ”down” ▼, choose the neededparameter to be entered;- by pressing “Enter” the cursor will mark the number to be changed. Forexample: FAT=01.29;- using the buttons “up” ▲and ”down” ▼, enter the needed value;- by next pressing of Enter pass towards the next number;- after completion of entering the needed FAT value, press Enter;- the cursor returns to its starting position.Cal 1 Samp.HighFat=f.ffSNF=y.yyDen=d.ddWith the button “down” ▼ move the cursor across SNF and analogical to theabove described consequence enter the value for SNF and after that the restof the values.Using menus Edit samp's 1(2,3) the operator has the possibility preliminaryto prepare the data for the parameters for each recalibration separately or tocheck the sample data.Operation manual 31/98

Ultrasonic milk analyzer6.4.2.3. Making recalibration with the available samplesAfter entering the values for the separate parameters of the sample positionthe cursor across Exit, press Enter and the following menu appears on thedisplay:Recalibrate 1Put sample High 5timeswhich reminds us to put 5 times the sample with high FAT.The sample has to be with temperature in the boundaries 15-25°С.Stir 2-3 times the milk sample before each measurement by pouring it fromone vessel to another. The needed quantity is poured in the sample-holderand it is put in the recess of the device. Starts the measurement. The sampleis sucked. Appears the following menu:Recallibrate 1Put sample high 5timesSamp T=16.8After the sample is measured, appears the following menu:Recalibrate 1Put sample HighCal meas=1/5which reminds to make the next measurement. Follow the procedure till the5th measurement.After 5th measurement completion automatically appears the menu:Operation manual 32/98

Ultrasonic milk analyzerCal 1 Samp LowFat = f.ffSNF=y.yyDen=d.dd------------------------------Lac=l.llSol=s.ssPro=p.ppExitWhich reminds to enter the values for the sample with low FAT. Enter thevalues analogically to the procedure, described in the previous sample. Afterentering the last parameter position the cursor on “Exit”, press “Enter” andthe following menu will appear:Recal 1Put sample Low 5timesMake 5 times measurement of the low FAT sample.After 5th measurement completion automatically appears the menu:Recal 1Put sample waterWhich reminds for 5-times water measurement. There is no need to entervalues after placing the sample-holder. Measurement starts directly.After the 5 th measurement appears the menu:RecalibratedAnalyzer readyThis means that the calibration was completed successfully and the analyzeris recalibrated for cow milk, marked as “Calibr 1”.Switch off the power supply of the device and switch it on again.The device is ready to work with the new calibration.If during work the sample’s temperature exceeds the temperature range 15-25° С the following message appears:Operation manual 33/98

Ultrasonic milk analyzerTemperature out ofrangeWait till the end of the measurement. When the message appears:Put sample againPut sample with temperature in the temperature range and continue themeasurement till completion of 5-time measurement.Operation manual 34/98

Ultrasonic milk analyzer7. STARTING THE DEVICE IN A SERVICE TEST/SETUPOPERATIONAL MODE. MENUS DESIGNATION7.1. Starting the device in a service Test/Setup operational mode.In order to start the Setup of the device the operator has to press the buttonEnter and without releasing it to switch on the power supply of the device, towait for the starting identification messages and to release the button afterthe following message appears on the display:Release buttonto start setupAfter releasing the button on the display is shown:MA SetupFollowed by possible to be entered by the operator menus:Special modesCorrectionsSettings------------------------------TestspH & Co MeterAccessoriesExitYou may move in the menus by using buttons “up” ▲ and “down” ▼.If by pressing the button Enter you choose a menu, each menu offers newpoints/submenus. When Exit is chosen the device leaves the Setup modeand returns to normal work.Operation manual 35/98

Ultrasonic milk analyzerDue to the continuous improvements made in the milk analyser or due to thetype of the ordered product, it is possible some of the options in the device tobe not active. In this case, if you try to enter the corresponding menu, thefollowing message will appear: Not available option.7.2. Menus Function:7.2.1. Special modes.Serve for choosing special (technological) working modes. After starting it thefollowing appears on the display:Special modesCalibrationCycleExitThis mode is normally used in production conditions.7.2.1.2. Calibration modeIn mode Calibration the analyzer is ready to make measurement and to sendthe received results towards the technological milk analyzers calibrationsystem. For this purpose you need personal computer type IBM PC,company’s calibration system LSC.EXE and methods for calibration of milkanalyzers (see the corresponding documents). To start measurement in thismode, the operator has to put a sample-holder containing milk sample in therecess of the analyzer and to press the button Enter.7.2.1.2. Cycle modeMode Cycle serves for training the analyzers. When you start this mode, theanalyzer, without additional commands, sucks the sample, makes themeasurement, pours the sample out in the sample-holder and displays thereceived results cyclically.7.2.2. CorrectionsServes for entering corrections in the measured data. Detailed description inpoint 6.3.2 and 6.3.3.Operation manual 36/98

Ultrasonic milk analyzer7.2.3. Settings.Serve for assigning different working parameters (modes).7.2.3.1. Net number.Serves for assigning the device network number when connecting it in theproduction network. The possible numbers are from 0 to 15 including.After starting this function the display shows the following:Net number0- OK +By using the button “up”▲ the operator has the possibility to increase thenumber, showing the channel’s number, and by button “down”▼, to decreaseit. Pressing the button Enter saves the chosen channel and exits the function.When connected in the production network each device has to have a uniquenumber.7.2.3.2. COM1 mode.Serves for choosing the working mode of COM1 (RS232 on the rear panel).Chooses the device towards which the measurement results are send. Thereare two possibilities:towards a personal computer - PC; towards serial printer - Prn.After staring this function the display shows the following:COM1 mode:Prn _PC OK PrnUsing the button “up”▲” the operator has the possibility to send the resultstowards Prn, and by button “down”▼, towards PC. Pressing the button Entersaves the chosen output device and exits the function.Forwarding the printer towards COM1 is necessary when connectingadditional external keypad to the analyzer. In this case the keypad isconnected to connector Printer, and the printer – to connector RS 232.Operation manual 37/98

Ultrasonic milk analyzerForwarding the printer could not be necessary if there is a special cable –fork-joint (from the company-producer), which allows both the keypad andserial printer to be connected towards connector Printer. I this case theconnector RS232 is free and may be used for communication with computerIBM PC type.7.2.3.3. LCD Setup.Serves to adjust the backlight of the display. This parameter may be changedin two modes:- fast – for rough adjustment;- fine – for precise adjustment.After starting this function the displays shows the following:LCD Setup:LCD SetupContrast fastContrast fineB. Light fast------------------------------B.Light fineExit7.2.3.4.Recalibrate.Serves for changing definite calibration. Methods are described in point 6.4.7.2.3.5. Edit FrPointThrough this menu you have the possibility to enter the basic freezing pointseparately for each calibration. For more information, see Appendix Freezingpoint . After choosing the menu the following is displayed:Edit FrPointsFrPoint Calibr1FrPoint Calibr2FrPoint Calibr3-----------------------------ExitOperation manual 38/98

Ultrasonic milk analyzerAfter choosing freezing point for the calibration, the following is displayed:FrPoint Calibrx-0.fff- OK +Where:Calibrx-0.fff- basic freezing point to be edited for chosen calibration.- basic freezing point current value.By pressing the buttons:“up”▲ - you may increase the absolute value of the freezing point”down”▼ - you may decrease the absolute value of the freezing point“Enter” - saves the edited value and exits the menu.7.2.3.6. Save/Rest Cal.Through this menu you may save the new calibration in the device or torestore the old one (factory) calibration. This is necessary in case that you’vecalibrated the device for cow milk, but after that the device is not measuringcorrectly and you decide to restore the factory calibration settings. Positionthe cursor across “Restore calibration” and press “Enter”Possibilities:Save calibration – saves the chosen calibration in an internal buffer.Restore calibration – restores the chosen calibration from the internalbuffer.The procedure Save/Restore is done for each calibration separately.Current workingcalibration (1,2 or 3)SaveInternal storingbufferCurrent calibration content is not changed, the analyzer continues using it,but there is a reserve copy in an internal buffer.Current workingcalibration (1,2 or 3)RestoreInternal storingbufferOperation manual 39/98

Ultrasonic milk analyzerThe current calibration is replaced with the calibration from the internal bufferand the analyzer starts working with it. The content of the internal buffer is notchanged.If after recalibration “Save calibration” is pressed the new calibrationsettings will be saved over the factory settings. After that is impossibleto restore the factory settings of the calibration. Save the newly madecalibration only if you are sure about its correctness.7.2.3.7. Settings Page 2.After this menu is started the display shows the following:Settings Page2Final clean CntAuto Print ResLarg Res En/DisSet Calibr NameExitNow there is a possibility one of the following options to be set:7.2.3.7.1. Final Clean CntSets the number of cleaning cycles.7.2.3.7.2. Auto Print Res.It is possible (if it is needed) to prohibit the automatic printing the measurementresults. If there is external keypad connected, then the results could be printedby pressing the button 1 from the keypad. It is possible to print out unlimitednumber of printouts for one and the same measurement.7.2.3.7.3. Larg Res En/Dis.The format of the measurement data send towards the computer is set.If the option Large Disable, is chosen, then only the main results are send tothe computer – Fat, SNF, Density, Lac, Proteins, Added Water, sampletemperature, device serial number and calibration number.If the option Enable, is chosen, except the above mentioned parameters alsodata for Salts, Freezing Point, pH, Conductivity will be send to the computer. Inthis case is necessary the software in the computer to be conformable to theformat of the sent data. After starting the menu, the display shows (for example):Operation manual 40/98

Ultrasonic milk analyzerLarge ResultsNoNo OK Yes7.2.3.7.4. Set Calibr Name.Sets the names of the separate calibrations. The name could be chosen fromthe group of predefined calibrations names or to edit a new one. When editingthe new name there is a possibility all ASCII codes to be used, as letters (capsand normal), numbers and punctuation marks and popular symbols. Thecalibration name consists of 8 symbols.After starting this menu the display shows:Select CalibrCal1: SheepExit Yes NextThere are the following possibilities:With button Exit – to leave the menu.With button Yes – to confirm the chosen for editing calibration name.With button Next – to choose the next calibration name for editing.If a calibration for change or edit of name is chosen, the display shows(example):Cal:SheepPreDef Exit EditThere are the following possibilities:With button PreDef – to choose a calibration name from the list of preliminarygiven names.With button Exit – to leave the menu.With button Edit – to edit the new calibration name.If a name from the preliminary given names list is chosen, the display shows:Operation manual 41/98

Ultrasonic milk analyzerCal1: SheepUHTExit Yes NextThere are the following possibilities:With button Exit – to leave the menu.With button Yes – to confirm the chosen from the list calibration name.Now theprogram returns to the beginning of the menu for setting calibration names.With button Next – to show the next calibration name from the list.If it is decided a new calibration name to be edited, the display shows:Cal1: SheepUser EditedName:Prev Set NextThere are the following possibilities:With button Prev – to display the previous ASCII symbol.With button Set – to confirm the ASCII symbol, shown on the display andpasses to editing the next symbol from the calibration name.With button Next – to show the next ASCII symbol.After editing the last (eighth) name symbol, the display shows:Cal1: SheepUser EditedName:MilkShpExit SaveThere are the following possibilities:With button Exit – to leave the menu.With button Save – to confirm already edited calibration name and to save it inthe device. The program returns to the beginning of the menu for settingcalibration names.7.2.4. Tests.Operation manual 42/98

Ultrasonic milk analyzerStart different tests. Possibilities:7.2.4.1. Test pump.Starts pump’s test. The number of the completed suction/display cycles isindicated.7.2.4.2. Ultrasound.Test for the ultrasonic system. Used in production conditions.7.2.4.3. Serial Prn.Display a short text of a serial printer, connected to COM2 – output withmessage Printer on the back panel of the device.7.2.4.4. Set Amplitude.Serves for ultrasound amplitude adjustment. It is used under productionconditions or by the customer (after sensor change) according theinstructions in the document SetCell.pdf.Please, use this menu only after reading the above pointed documentSetCell.pdf7.2.5. pH meter & Co meterPh and conductivity measuring are additional possibilities for the analyserand are optional. Their usage is described in Appendices PH Measuring andConductivity Measuring.7.2.6. ExitBy pressing the button you may leave the program and pass towards anothermenu.7.2.7. Milk analysers’ setup menu structureSpecialmodesCorrectionsCalibrationCycleReportsShut DownAnalyzer SetupOperation manual43/98

Ultrasonic milk analyzerSettingsCalibration 1Calibration 2Calibration 3TemperatureCondmeasureNet numberCOM1 modeLCD SetupRecalibrateEdit FrPointsSave/RestCalFatSNFDensityLactoseSaltsProteinsWaterFatSNFDensityLactoseSaltsProteinsWaterFatSNFDensityLactoseSaltsProteinsWaterContrast fastContrast fineB.Light fastB.Light fineCalibration 1Calibration 2Calibration 3Edit samp's 1Edit samp's 2Edit samp's 3FrPoint Calibr1FrPoint Calibr2FrPoint Calibr3Save Calibr 1Save Calibr 2Save Calibr 3Operation manual44/98

Ultrasonic milk analyzerFan TempOffsSettingsPage2Rest Calibr 1Rest Calibr 2Rest Calibr 3Final clean cntAuto Print ResLarg Res En/DisSet Calibr NameOption SelectSel Pump SpeedSpeed for Cal 1Speed for Cal 2Speed for Cal 3HFSpeed for CalOutSample DelayResltPrecisionPropertiesFat - PrecisionSNF - PrecisionDen - PrecisionLac - PrecisionSol - PrecisionPro - PrecisionAdW - PrecisionTestspH & CoMeterTest pumpUltrasoundSerial PrnterKeyPadDisplaysParallel PrnpHCalibrationpHMeasuringpHEn/DisablepH U DisplaypH Test U[V]Co MeterCalibrPCB Main IdentiPCB LCD IdentiOperation manual45/98

Ultrasonic milk analyzerAccessoriesCo MeterTestCo MeterEn/DisWeight scaleBatteryRT ClockRaw TestCalibrationMeasureOn Line En/DisMeasure Bat UCtrl Enabl/DisDisplay TimeAdjust TimeAdjust DateOperation manual46/98

Ultrasonic milk analyzer8. ADDITIONAL POSSIBILITIES OF THE ANALYZER8.1. Connecting to 12 V DC power supply.If there is a need the analyzer to work on place without electrical supplyavailable, then it could be powered by car battery or other 12 V DC externalpower supply. Use the 12 V power supply cable (art. number 90-1801-0009,Parts and Accessories, point 15).8.2. Connecting to IBM PCThe milk analyser can be connected to IBM PC using the RS232 interfacecable (art. number 90-1801-0010, Parts and Accessories, point 16). In orderto make the connection: switch off both milk analyser and PC.Connect the RS232 cable towards Serial interface and towards the computer. Turn on bothmilk analyser and PC. Now the milk analyser is ready to communicate withIBM PC.8.3. Connecting a printer (option).In order to print out the measurement results, a serial printer could beconnected to the device – for example ESC/POS Serial printer, production ofDatecs or Seiko. The interface connector for the printer is on the rear panel ofthe device - “Serial printer output”. The printer (if it is Datecs), should beconnected to the “12 V printer output” on the device rear panel. Connect it viacables, delivered by the company-producer. If the printer is connected directlyto the electrical network, then the analyzer and the printer should beconnected to one and the same electrical phase.Communication parameters: 9600 bps, No parity, 8 bits, 1 stop bit. It’s onewaycommunication (uses one line) – the analyzer only sends and the printeronly accepts data.8.4. Connecting and working with external keypad (option).It is possible external keypad (supplied by the producer of the device) to beconnected to the device, using special cable to the serial printer connector.In order to connect external keypad to the milk analyzer, follow the procedurebelow:1. Connect the keypad towards connector labeled Printer.2. Connect the printer towards connector labeled RS 232.3. Forward the printer towards output RS 232, doing the following:1. Press the button Enter (on the front panel of the analyzer).2. While holding it pressed, switch on the analyzer’s power supply.3. Release the button Enter.4. Using the buttons Up/Down choose menu Settings and pressEnter.Operation manual47/98

Ultrasonic milk analyzer5. Using the buttons Up/Down choose menu COM1 Mode andpress Enter.6. With the right button (Up) choose COM1 Mode – Prn, pressEnter and leave the menu.With the external keypad 4 digit identification number of the milk deliverermay be entered (from 1 to 9999) and quantity of delivered milk in liters (from0,1 to 9999.9) (accurateness up to 0.1 l). These data entering have to becompleted before starting measurement. Pressing the button Enter on thekeypad will display the following:Enter DataDel N:Now enter the deliverer’s identification number. After pressing Enter on theexternal keypad, the display shows:Enter DataDel N:xxxxLiters =Now, enter how many liters have been delivered and press the button Enteron the external keypad the following is displayed:Del N:xxxxLiters=yyyy.yAre you sure?0-No Yes-EnterWhere:хxxxyyyy.y- entered by the operator identification number of the deliverer- entered by the operator liters.The operator has two possibilities:1.To cancel the entered data by pressing the button 0 on the external keypadand to start entering them again.2.Confirm the entered data by pressing the button Enter on the externalkeypad. The display shows currently chosen calibration. The device is readyto start measurement. After completing the measurement, the data for thedeliverer are printed out.Operation manual48/98

Ultrasonic milk analyzerAPPENDICESAPPENDIX 1 METHODS1. Determination of milk's density1.1. GeneralMilk density is defined as relation between the mass of definite milk volume attemperature 20 o С and the mass of equal volume distilled water attemperature 4 o С.Density, alone, could not be used as a control parameter at milk qualitycontrol. Using the density the tentative figures for the SNF and salts could bedetermined.1.2. Sampling and preparation for analysesSampling milk or other milk derivatives and their preparation for analyses isdone according corresponding Appendices.Milk density is determined not earlier than 2 h after milking. The milk must bewith temperature from 10 to 25 o С.Before determination of density the milk must be well stirred. To avoid foamformation, it has to be carefully poured on the cylinder’s walls. The cylindermust be slightly tilted.Before taking the readings the cylinder, with the milk must be placed on aneven surface, facing the light, so the readings could be easily seen.1.3. Basic principles.The density of the milk is determined using aerometer, also called lactodensity-meter(milk density meter) and is expressed with a number,representing milk density meter degrees, decreased 1000 times or only withmilk density meter degrees.1.4. Necessary devices and reagents- Aerometer /lacto-density-meter, milk meter/.- Cylinder – with inner diameter not less than 5 сm, and length, correspondingto the dimensions of the lacto-density-meter.- Ammonium with preliminary defined relative density.1.5. Making the determination:Dry and clean, the lacto-density-meter is slowly dipped in the milk till division1,030, and then is left in free-floating state. The lacto-density-meter must nottouch the cylinder’s walls and to be on at least 5 mm from them.When taking the readings the eyes must be on one and the same level withthe meniscus. The reading is done in the meniscus’ upper end with accuracytill 0,0005, and the temperature – with accuracy till 0,5 o С.Operation manual50/98

Ultrasonic milk analyzerThe difference between two parallel determinations must be not more than0,0005.1.6. Recalculating the values according lacto-density-meter at 20 oС.If the milk, when determining its density, has temperature, higher or lowerthan 20 o С, the readings from lacto-density-meter are recalculated towards 20o С.Density recalculation towards 20 О С is done on the following way:for every temperature degree over 20 О С from the received by the milkmetervalue are added 0,2 o for the cow and goat milk and 0,25 o for sheep andbuffalo milk lacto-density-meter degreed or 0,0002, respectively 0,00025towards density; and for every temperature degree under 20 o С from thereadings of milkmeter value are deducted 0,2-0,25 lacto-density-meterdegrees or 0,0002, (0,00025) from the density.2. Determination of fat content in the milk and milk derivatives.2.1. GeneralFor making analyses are used pure reagents for analyses (pure reagents foranalyses (p.r.a.) and distilled water or water with equivalent purity.2.2. SamplingMilk and milk derivatives sampling is done according Appendices Milksampling and preparation of samples for analyses ad Sampling andpreparation of samples for verification the accuracy of the milk analyser,making corrections and recalibration.2.3. Basic principles.The method uses dissolving the milk and dairy products proteins withsulphuric acid with definite concentration in butyrometer and separating thefat under the influence of amilic alcohol, heating and centrifuging in a form ofdense transparent layer, the volume of which is measured in the graduatedpart of the butyrometer.2.4. Necessary devices and reagents• Butyrometers for milk, special for skimmed milk and cream;• Rubber stopples for butyrometers;• Stand for butyrometers;• Special pipettes or automatic for milk, sulphuric acid and изоамиловalcohol from 1, 10 and 11 сm 3 ;• Pipettes from 1 and 20 сm 3 ;Operation manual 51/98

Ultrasonic milk analyzer• Glasses from 25 till 50 сm 3 ;• Centrifuge for Gerber;• Water bath;• Mercury thermometers up to 100 o С with value scale 1 o С;• Sulphuric acid with density 1,82 at 20 o С for determination of fat contentof the milk;• Isoamilic alcohol for Gerber with density 0,811 to 0,812.2.5. Making the determination:Preparation of samples for analyses.The milk is mixed well in order to become homogenous mixture (if necessaryit is slowly heated up to 35-40 о С ) and is carefully shaken and tempered to20±2 о С. The samples from whey and buttermilk are preliminary filteredthrough double layer gauze and is then tempered to 20±2 о С. Cream samplesare placed in water-bath at temperature 35 till 40 о С, stirred till homogenoussample is received and cooled down to 20±2 о С.2.6. Making measurementWith butyrometer for milkFor milk, whey and buttermilk.With automatic or special for acids pipette are measured 10 сm 3 sulphuricacid with d=1,820 кg/m 3 at 20 о С in the milk butyrometer. Carefully on thebutyrometer's walls are piled up 11 сm 3 from the prepared sample. Thepipette is held till its full drainage.For creamFrom the prepared sample is measured 10 g with error up to 0,001 g and 50сm 3 water are added. Mixture is well stirred and heated up to 30-35 о С, thenis again stirred and cooled down to 20±2 о С, and the following steps are aswith the milk sample using sulphuric acid with d=1,789 till 1,790 кg/m 3 .With butyrometer for creamFor cream5 g from the sample are measured with butyrometer with error up to 0,0001 gand then 5 сm 3 water are added, 10 сm 3 sulphuric acid with d=1,780 to 1,790кg/m 3 at 20 о С and 1 сm 3 изоамилов alcohol. The butyrometer is closed withrubber stapple and is shaken till the proteins are fully dissolved.2.7. Calculating the resultsBy using milk butyrometerMilk, whey, buttermilk.Using the butyrometer's graded scale the grams fat in 100 g product are readdirectly. When the milk is curdled, the result is increased with 0,1 g for everydegree.By using cream butyrometer.Operation manual 52/98

Ultrasonic milk analyzerCreamUsing the butyrometer's graded scale the fat content in the products isdirectly read in percentages.2.8. Measurement accuracyBy using milk butyrometerThe difference between two parallel determinations could not exceed:For skimmed milk, whey and buttermilk - 0,05 g for 100 g product;For cream - 0,5 g for 100 g product;For milk - 0,1 g for 100 g product;By using cream butyrometerThe difference between two parallel determinations could not exceed 0,5 gfor 100 g cream.3. Determination of water content and solids in the milk and milkderivatives.3.1. GeneralThe solids represent the fat content, proteins, carbohydrates and salts.Sampling is done according Appendices Milk sampling and preparation ofsamples for analyses ad Sampling and preparation of samples for verificationthe accuracy of the milk analyser, making corrections and recalibration.3.2. Basic principles.Water content is determined by weight when drying at temperature (102±2)о С of the weighted product till constant mass, expressed in grams for 100 gproduct.The solids/dry substance is the mass of the dry remainder, received afterdehydration of determined quantity product at temperature (102±2) о С tillconstant mass and is expressed in grams for 100 grams of the product.3.3. Necessary devices and reagents- Assay balance with loading bounds 200 g and error 0,0002 g.- Mercury thermometers from 0 to 100 О С and from 0 to 150 o С with value ofscale division 1 o С;- Pipettes from 5 to 10 сm 3 , class II;- Glass banks with grind stopples with volume 100-200 сm 3 ;- Drying-oven with thermal regulator for keeping the temperature (102±2) o С;- Exicator with silicagel or another hygroscope material;- Weight plates;- Peg for the weight plates;- Glass pods with rounded ends;- Quartz, sea or river sands.Operation manual 53/98

Ultrasonic milk analyzer3.4. Making the determination:Sample preparation for analyses.The milk (whey, cream, and buttermilk) is well shaken. If needed, the sampleis heated slowly up to 38-40 о С, it is well mixed and cooled down to 20 о С.Mixing and pouring are done at least three times in dry and clean vessel.3.5. Making the measurementThe weight plate with 20-30 g washed out and tempered sand and glass rodis dried at 102±2 о С for 1 h, and then is taken out, covered with the cap,tempered with exicator (up to 30 min) and the mass is weighted withaccuracy up to 0,0005 g. In the weight plate, using pipette, at about 10 сm 3milk are poured, covered and weighted. With the help of the glass rod milk iswell mixed with the sand and without a cap is heated on a water-bath till ahomogenous mass is formed. Then the weight plate is put in a drying-oven attemperature 102±2 о С, it is dried out for 3 h, it is taken out of the oven,covered with the cap, tempered in exicator (up to 30 min) and the mass isweighted. Weight-glass is placed in the drying-oven again and is dried 1 h,then is taken out, tempered and weighted. This procedure is repeated till thedifference between two consequent measurements becomes not more than0,004g. In case that at the second or following drying procedure massincreases, then for the calculation is taken the previous measurement.3.6. Calculating the resultsWater content in grams for 100 g product (milk or milk derivatives), iscalculated by the formula:M2− M3X = ∗100M2− M1WhereМ1 - the mass of the plate with the sand and the glass rod, g;М2 - the mass of the plate with the sand, the glass rod, and the samplebefore drying, g;М3 - the mass of the plate with the sand, the glass rod, and the sample afterdrying, g;The dry substance (Y) is calculated using the formula:Where:Y= 100 - Х,Х is the calculated water content.3.7. Measurement accuracy.Operation manual 54/98

Ultrasonic milk analyzerThe difference between tow consecutive measurements of one and the samesample could not be more than 0,2 g for 100 g product.4. Determination of casein content in the milk.4.1. GeneralThe methods are based on the Volker's method.For making the analyses are used pure reactive for analyses (p.r.а.) anddistilled water or water with equal purity.4.2. SamplingAccording corresponding Appendices.4.3. Basic principles.Added to the milk formalin liberates acidic residuum from the protein's endgroups, which are titrated with soda caustic solution. The soda causticquantity is proportional to the casein in the milk content.4.4. Necessary devices and reagents- Glass 250 сm 3 .- Pipettes Foll - 25,5 сm 3 .- Pipettes Mor from 1 сm 3 , with division 0,1 сm 3 .- Soda caustic p.r.а. - 0,143 n solution.- Formalin 40% p.r.a - freshly neutralized.- Phenolphthalein - 2 % solution in 70 % ethyl alcohol.- Potassium oxalate p.r.а. 28 % water solution.- Cobalt sulphate p.r.а. 5 % water solution.4.5. Making the determination:For cow milkReference sample preparation.20 cm 3 from the measured milk are poured in a glass vessel together with 1cm 3 3 % water solution of cobalt sulphate. The sample is shaken and a slightrose color of the solution is received, which serves as a standard in theresearch.4.6. Making the measurement20 cm 3 from the milk are measured in a glass and a titrated with 0,1 N sodacaustic, using phenolphthalein as an indicator, till the color of the standardsample is reached. The volume of the used soda caustic is not taking intoconsideration.4 cm 3 38-40 % formalin are added towards the neutralized sample and therose color disappears as a result of the liberated carboxylic groups. It is wellOperation manual 55/98

Ultrasonic milk analyzerstirred and titrated with 0,1 N soda caustic, till slight rose color is recovered.At the second titration the volume of the used soda caustic is measured.For sheep milkCasein content in sheep milk is determined on the same way. The onlydifference is that instead of 4 cm 3 38-40 % formalin in the milk are added 6cm 3 , and the standard/reference sample is prepared with 1 cm 3 4 % solutionof cobalt sulphate.4.7. CalculationsThe quantity of the 0,1 N soda caustic in cm 3 , used in the second titration,multiplied by the coefficient 0,7335 is equal to the casein content in the milkin percentages.The following tables could be used for quicker readings of casein'spercentage on the base of used cm 3 0,1 N soda caustic:Table ICalculation of casein content in the cow milk on the base of used cubiccentimeters 0,1 N soda caustic:0,1 n NaOH cm 3 Casein% 0,1 n NaOH cm 3 Casein % 0,1 n NaOH cm 3 Casein %3,00 2,20 3,35 2,46 3,70 2,713,05 2,24 3,40 2,49 3,75 2,753,10 2,27 3,45 2,53 3,80 2,793,15 2,31 3,50 2,56 3,85 2,823,20 2,35 3,55 2,6 3,90 2,863,25 2,38 3,60 2,64 3,95 2,903,30 2,42 3,65 2,68 4,00 2,93Operation manual 56/98

Ultrasonic milk analyzerTable IICalculation of casein content in the sheep milk on the base of used cubiccentimeters 0,1 N soda caustic:0,1 n NaOH cm 3 Casein% 0,1 n NaOH cm 3 Casein % 0,1 n NaOH cm 3 Casein %5,40 3,96 6,10 4,47 6,80 4,995,45 4,00 6,15 4,51 6,85 5,025,50 4,03 6,20 4,55 6,90 5,065,55 4,07 6,25 4,58 6,96 5,105,60 4,10 6,30 4,62 7,00 5,135,65 4,14 6,35 4,66 7,05 5,175,70 4,18 6,40 4,69 7,10 5,215,75 4,22 6,45 4,73 7,15 5,245,80 4,25 6,50 4,77 7,20 5,285,85 4,29 6,55 4,80 7,25 5,325,90 4,33 6,60 4,84 7,30 5,355,95 4,36 6,65 4,88 7,35 5,396,00 4,40 6,70 4,91 7,40 5,436,05 4,44 6,75 4,95 7,45 5,464.8. Measurement accuracy.Two parallel samples are measured and the difference between them couldnot exceed 0,1 %.The accuracy of the method require the work to be done at place with goodnatural illumination, titration to be done evenly, without interruptions, colorlessformalin to be used, preliminarily neutralized with soda caustic andphenolphthalein indicator.Formalin titration is easy method, but it is not enough precise. More accurateresults for casein content are obtained using Kjeldhal's method, but it requiresspecial appliances.5. Determination of salts in the milk5.1. GeneralFor the mineral substances in the milk conclusions can me made on theashes content.5.2. SamplingAccording Appendices Milk sampling and preparation of samples for analysesad Sampling and preparation of samples for verification the accuracy of themilk analyser, making corrections and recalibration.Operation manual 57/98

Ultrasonic milk analyzer5.3. Basic principles.Milk is dried, carbonized and turned to ashes till constant mass. The ashesreceived are calculated in percentages.5.4. Necessary devices and reagents• Assay balance;• Crucibles;• Water-bath or infrared lamp;• Hot plate or burner;• Drying-oven with thermal regulator;• Muffle furnace;• Exicator;• Quantity filter.5.5. Making the determination:In preliminary tempered and weighted crucible of the assay balance at about10 g milk is weighted with accuracy up to 0,0005 g. The crucible with thesample is placed in a water-bath or infrared lamp till the evaporation of milk todry state. Then it is carbonized with the burner or on a hot plate, payingattention not to be splashed out. The crucible is placed in a muffle oven andturns to ashes slowly, without the sample to be kindled, at temperature 500-550 о С till white or grey-white ashes. It is tempered in an exicator and isweighted till the appointed accuracy. Heating up in the oven is repeated till aconstant mass is received.5.6. CalculationsAshes content is calculated using the formulaashes =( C( B−−A)∗100A)Where:А – the mass of empty, tempered crucible, gВ – the mass of the crucible together with the milk, gС – the mass of the crucible with the received ashes, g5.7. Measurement accuracyThe difference between tow parallel determinations could not be more than0,02 %.Operation manual 58/98

Ultrasonic milk analyzerAPPENDIX 2 REPRESENTATIVE SAMPLES FROM MILK ANDOTHER MILK DERIVATIVES FOR MILK ANALYSER’SCALIBRATION1. GeneralThe samples used for analyser’s calibration have to be representative for thecorresponding milk type and have to be with known quality parameters: fat inpercentage, SNF in percentage, density, lactose in percentage, total proteinin percentage and salts in percentage. Changes in the analyzed parametersin the samples have, if possible, to cover the whole measuring range – i.e.used samples to be with low, middle and high content of the analyzedcomponents.The exact value of the parameters is decisive for correct and accuratecalibration, because if the parameters are not set correctly during calibrationthe same parameter will not be measured correctly.2. Necessary quality parameters values determinationFor more precise determination of above listed quality parameters of the milkand its derivatives is advisable they to be examined in an authorizedlaboratories, using the corresponding arbitration methods for this purpose.2.1. Laboratory methods2.1.1. Determination of fat contentDetermination of fat content in the milk and its derivatives (cream, whey,buttered milk) is one of the most important analyses in the dairy productionand milk processing. According this parameter the payment schemes aremade and it is observed from the point of view correct production processand the basic economy balances are made with its help.А/ Röse-Gottlieb methodThe fat content is determined using the gravimetric method, fat extractionfrom ammonia-alcohol milk solution using diethyl and petroleum ether,evaporation of the solvent and weighting the residuum.B/ Gerber methodThe proteins in the milk and dairy products are dissolved with sulphuric acidwith definite concentration in butyrometer and the fat is separated under theinfluence of amyl alcohol, heating and centrifuging in a form of dense,Operation manual 59/98

Ultrasonic milk analyzertransparent layer. The volume of this layer is measured in the divided part ofthe butyrometer.This is quick, easy method with sufficient accuracy. We recommend it forusage. For more detailed description see Appendix Methods.2.1.2. Milk density determinationА/ With picnometer and Mor-Vestval scalesThis is the most exact method for determination of milk and its derivatives’density.B/ with aerometer (lacto-density-meter)Compared with the above method this is quick and easy readable withsatisfactory accuracy. We recommend it. For more detailed description seeAppendix Methods.During the lactation period and under the influence of different zooengineering factors the density of the different milk kinds varies in thefollowing bounds:Milk kind Minimum Maximum AverageCow 1,027 1,033 1,030Buffalo 1,026 1,032 1,029Goat 1,027 1,033 1,030Sheep 1,031 1,040 1,0342.1.3. Determination of total proteinsА/ Kjeldahl methodHeating with concentrated sulphuric acid in the presence of catalystmineralizes a definite volume of the milk sample. The liberated ammoniumcombines with the sulphuric acid and forms ammonium sulphate. After addingsurplus soda caustic ammonium is liberated. When distilled it combines withthe boronic acid. The quantity of the combined ammonium is determined bytitration with acid with determined titer. From the combined with theammonium acid the initial nitrogen content is determined, and also theproteins in the milk.B/ Titration with formalinFormalin, added to the milk, combines with the amino group in the protein’smolecule and forms methyl groups, which have no alkaline reaction. Milkacidity increases by the liberated carboxylic groups, which are titrated withsoda caustic solution. The used volume soda caustic is proportional to theprotein content in the milk.Operation manual 60/98

Ultrasonic milk analyzer2.1.4. Determination of casein content in the milkА/ Kjeldahl methodThe total nitrogen content in the milk is determined. Casein is precipitatedwith acetic acid (acetate buffer) and is filtrated. The content of nitrogen in thefiltrate is determined. Casein content is the difference between the two resultsfor nitrogen using the Kjeldahl’s method.B/ Titration with formalinMore details for this method – see Appendix Methods.2.1.5. Determination of salts in milk.For the salts in milk and its derivatives is judged by its ashes content. Milkdries, becomes carbonized and turns to ashes till constant mass. The ashesreceived are calculated in percentage.2.1.6. Determination of solids in milkSolids describe the content of fats, proteins, carbohydrates and salts. Itsvalue may be used for determination of each of these parameters in case ofknown other values.Salts are determined by drying till constant mass – see Appendix Methods.Express methods by using another milk analysersIt is possible another device to be used for determination of some of thequality parameters of milk and its derivatives samples, intended forcalibration, but it has to be noted that it is possible incorrect values to bereceived, that’s why it is necessary to be completely sure in the accuracy oftheir readings.Usage of Milkoscan and other milk analysers based on the infraredmeasurement principle.By using it the fat, lactose and protein content may be determined. Problemmay arise with determination of salts and SNF. This is due to the impossibilityof the infrared method to determine the solids and in order to receive thesolids in the sample their meaning is accepted as a constant.Operation manual 61/98

Ultrasonic milk analyzerAPPENDIX 3 MILK SAMPLING AND PREPARATION OFSAMPLES FOR ANALYSES1. GeneralMilk sampling and qualification of raw, thermally treated milk and itsderivatives (cream, whey, buttermilk etc.) is accomplished for every separatehomogeneous batch. As homogeneous batch is accepted:• Milk, delivered by a separate producer (an individual farm, farm etc.),and received from one kind of animals after their complete milking,independently from the number of milk-cans and tanks.• Milk, received from one or several farms or milk collecting centers, butdelivered in a joint vessel.• In the enterprise – from one and the same kind raw milk poured in onevessel.• For cream, whey, buttermilk etc. – produced as a result of milkprocessing and its derivatives from one and the same kind and quality,poured in a separate vessel.Milk is qualified not earlier than 2 hours after milking.When the milk is frozen it has to be warmed up to 10-15 o С and stirredaccording the below-described procedure.A sample is taken from every separate vessel proportionally to the quantity ofthe milk in it. Samples from the different vessels are mixed well and from thereceived medial sample are taken 200 - 250 cm 3 for accomplishing theneeded analyses.2. Stirring the milk and its derivatives before samplingMilk stirringIt is a very important condition for receiving exact results. Before takingsamples from big vessels the milk (fresh or thermally treated, whole-milk orwhipped) has to be well stirred for no less than 5 min., by vertical and circularslow movements. Mixing spoon with long handle is used, allowing the lowestlayers of the liquid to be reached.The milk in the milk-cans is stirred 5 to 8 times from the surface to the bottomand reverse with slow circular movements.Cream stirringDue to the fact that the cream is significantly thicker liquid than the milk andcontains high percentage fat it has to be preliminary very well stirred from thesurface to the bottom with reciprocation movements at about 20-25 times.Whey and buttermilk stirringIt is analogical to milk stirring.Operation manual 62/98

Ultrasonic milk analyzer3. SamplingSamples from milk, whey or buttermilk are taken with metal or glass pipe (dry,clean and stainless-steel) with diameter at about 10 mm, which is slowlydipped till the bottom of the vessel and its upper end remains open. In thisway it is filled with milk simultaneously with its dipping. When the pipe istaken out of the vessel its upper end has to be tightly closed with a thumb.For a bigger reliability of the analyses results it is recommended the quantityof the taken sample to be no less than 200 ml.Cream sample is carefully well stirred in order not to form foam. For taking amedial sample from milk-cans and tanks a sample pipe is used. Stuck to itsouter surface cream has to be removed by using filter paper, napkin or cleancloth, preventing in this way the proportionality between the samples and thetotal amount of the cream to be disturbed.4. Sample preservationThe vessels where the samples will be put have to be clean, dry, glass, metalor from other suitable material, to be tightly closed with rubber or otherstopples. The stopples not to absorb water and fat and not to influence theanalyses sample content.In summer the sample fills up to the top the vessel, but in winter – at least 3/4from the vessel’s volume. Each sample for analyses has to be labeled anddescribed in a way not allowing to be mixed up.The samples are stored in conditions, assuring temperature, corresponding tothe requirements for storing such kind of product (advisable – 1 o С).If there is a need of longer sample storing they have to be preserved; themost commonly used preservative is potassium dichromate (K 2 Cr 2 O 7 ) - 1 gfor 1 000 ml. The samples have to be stored in a cold and dark place after thepreservation. Have in mind that during the analyses the results for SNF% willbe increased with 0,1 %. After adding the preservative the sample has to bewell stirred.Do not make analyses if the acidity of the milk is more than 25 o T for cow and28 o T for sheep milk.5. Preparing the samples for analysesMilk – raw and thermally treatedOperation manual 63/98

Ultrasonic milk analyzerWhen examining samples taken immediately before analyses and shortlystored, the milk is poured several times from vessel to vessel in order todistribute the fat content uniformly. To avoid foam formation or separation ofmilk fat, the samples have to be carefully poured using the walls of thevessels, as they are tilted slightly. For a better mixing the sample it has to bepoured at least 3 times. When needed the same is tempered to thetemperature within the measuring range.If there is fat stuck on the walls of the vessel and the stopple (when thesamples were stored for a long time), the milk has to be slowly heated up to35-40 o C. At the same time it has to be slowly shaken. The cream, stuck tothe walls of the vessel is removed. The sample is poured several times and iscooled down (advisable up to 20 o С).If there is separated liquefied fat or white particles with irregular form on thevessel’s walls reliable results could not be received.WheyBefore making analyses the whey sample is filtered through double sheetgauze put over the glass funnel in order to separate the fat grains get intoliquid by incidence and if it is needed the sample is tempered and carefullystirred.ButtermilkBefore making analyses the buttermilk sample is filtered through single sheetgauze put over the glass funnel in order to separate the big protein particlesand if it is needed the sample is tempered and carefully stirred.CreamThe sample is slowly warm up to 35 – 40 o С in water bath. The fat isdispersed wholly by carefully shaking and if necessary, by stirring with glassstick. The sample is poured from vessel to vessel several times and is cooleddown (advisable to 20 o С). If after this procedure the sample is nothomogenous, the measurement is not carried out.Sample for analyses is prepared from homogenized cream by diluting it withdistilled water in degree, sufficient for the components of the diluted cream tobe reached in the measuring range of the analyser.Operation manual 64/98

Ultrasonic milk analyzerAPPENDIX 4 SAMPLING AND PREPARATION OF SAMPLESFOR VERIFICATION THE ACCURACY OF THE MILKANALYSER, MAKING CORRECTIONS AND RECALIBRATION.1. Necessary consumables and devices• Distilled water;• Minimum 3 milk samples with known content of fat, SNF, protein,density, lactose, solids;• Heating water bath;• Cooling water bath or chamber;2. GeneralMilk sampling and storage of samples of raw, thermally treated milk and itsderivatives (cream, whey, butter-milk etc.) aiming verification the accuracy ofthe analyser, making corrections and recalibration is accomplished followingthe recommendations below:• Sample to be taken from homogeneous batches, observing all therequirement;• The sample’s volume to be enough for making minimum 5measurements for each sample or not less than 0.5 l;• The samples to correspond to the standard physic-chemical andmicrobiological requirements, to be pure, without admixtures, withoutadded cleaning or other unusual substances and without falsifications;• Do not use samples with total acidity of milk more than 17 o T;• Vessels, where the samples will be handled have to be clean, dry,glass, metal or other suitable material, to be tightly closed with rubberor other stopples. The stopples not to absorb water and fat and not toinfluence the analyzed sample content;• Till the start of the analyses the samples are stored in conditions,assuring preservation of their content and quantities (advisable lowtemperature – 1-3 o С).For longer storage of the samples a preservative is added as was alreadydescribed in p.9.1.1, and then the sample has to be well stirred.3. Representative SamplesThe samples have to be representative for the corresponding milk type.Changes in the analyzed parameters in the samples have, if possible, tocover the whole measuring range – i.e. used samples to be with low, middleand high content of the analyzed components.Operation manual 65/98

Ultrasonic milk analyzerExemplary recommended values:Cow milkParameter Low value High value% fat content 2,00 6,00% Solids-Non-Fat content 8,00 9,00The Lactose percentage content (4,0-5,5; average-4, 7), Protein (2,00-4,00;average-3, 3), salts (0,7-0,8) is proportional to the SNF content. Whenpreparing samples these values vary within limited bounds.Sheep milkParameter Low value High value% fat content 5,50 10,00% Solids-Non-Fat content 9,00 11,50The Lactose percentage content (average - 4,6), Protein (average - 5,8), salts(average - 1,0) is proportional to the SNF content. When preparing samplesthese values vary within limited bounds.Buffalo milkParameter Low value High value% fat content 5,50 10,50% Solids-Non-Fat content 9,00 11,00The Lactose percentage content (average - 4,7), Protein (average - 4,3), salts(average - 0,8) is proportional to the SNF content. When preparing samplesthese values vary within limited bounds.Goat milkParameter Low value High value% fat content 2,00 6,00% Solids-Non-Fat content 8,00 9,00The Lactose percentage content (average - 4,6), Protein (average - 3,7), salts(average - 0,8) is proportional to the SNF content. When preparing samplesthese values vary within limited bounds.Operation manual 66/98

Ultrasonic milk analyzerCreamParameter Low value High value% fat content 8,00 20,00% Solids-Non-Fat content 2,50 5,00The cream samples are diluted with distilled water. Degree of dilution is 2-3times, in dependence of the initial fat content in the cream.WheyParameter Low value High value% fat content 0,20 0,80% Solids-Non-Fat content 5,00 7,50The content of fat and SNF in the whey depends on the kind of the dairyproduct as a result of which the whey is received.4. Samples preparationMilk – raw or thermally treatedFor raw milk sample with average content of the analyzed components isadvisable to be used milk, collected from at least 10 animals from the mostcommonly met breed in the region where the analyser will be functioning.Low fat and high fat samples are prepared on the following way:Available fresh or thermally treated milk is poured in a separating funnel,which is place in a refrigerator for at least 12 hours at temperature 4 - 6 °С inorder to stratify. For a bigger stratification a longer time is required.The layer at the bottom is poured in a vessel. It is well mixed by pouring itfrom vessel to vessel and is warmed up to 40 °С in a water bath.The upper layer is poured in another vessel.Using the certified methods the density and the concentration of the analyzedcomponents - fat, protein, SNF, lactose, salts are determined.The analyzer’s accuracy depends only on the correctness of the chemicalanalyses of the components in the samples and the normal acidity duringcalibration!It is recommended the first cow milk sample with low fat content to be withthe following parameters:Operation manual 67/98

Ultrasonic milk analyzer1.8-2% FAT; 8.7-9% SNF; 3,3-3,5 % Protein; 4,8-4,9% Lactose; 0,75 Solids;1030-1033 kg/m 3 Density.The second cow milk sample with high fat content to be with the followingparameters:5-5,5% FAT; 8.4-8,79% SNF; 3,1-3,2% Protein; 4,6-4,7% Lactose; 0,7 Solids;1028-1029 kg/m 3 Density.Samples with medial values of the separate parameters are received bymixing the two boundary values in a definite proportion.Preserve the samples, using above described method for their longerstorage.When using samples, stored shortly, preliminary pour the sample from onevessel to another in order to distribute the milk components evenly payingattention not to form foam in the sample.When the samples are stored for a longer period it is recommended to warmit up to 35-45 °С, and the vessel to be shaken carefully. In case that there is acream stuck on the vessel’s surfaces – remove it. The sample is poured fromvessel to vessel several times and is cooled down (advisable to 20 °С /.If there is separated liquefied fat or white particles with irregular form on thevessel’s walls this sample could not be used.Whey and buttermilkThe samples are poured several times from vessel to vessel and if neededgradual heating with stirring with cooling down is done.CreamThe sample is slowly warmed up to 35 – 40 °С in water bath. The fat isdispersed wholly by carefully shaking and if necessary, by stirring andpouring it from vessel to vessel till its full homogenization.From homogenized cream is prepared sample for analyses by diluting it withdistilled water in degree, sufficient for the components of the diluted cream tobe reached in the measuring range of the analyser.5. Advisable scheme for independently determination the content ofdifferent parameters in milk and its derivativesWhen is not possible to use the help of authorized laboratories and abovementioned milk analysers we recommend you to follow the scheme:Operation manual 68/98

Ultrasonic milk analyzer5.1. For cow milk (whole milk, low fat, skimmed milk) and UHT milkDetermination of fat content – Gerber’s method, described in AppendixMethods.Density determination – using aerometer, described in Appendix Methods.SNF determination – by formula – p. 3.2.3.1.BDetermination of Lactose content – by formula – p.3.2.3.2.АDetermination of salts content – by formula – p. 3.2.3.3.АTotal protein content determination – by formula – p. 3.2.3.4.АExample: Determination of the quality parameters for two samples cow milk(low fat and high fat), obtained and prepared according p. 2.3.1 and 2.4.1.First – determine the fat content in the samples, using the Gerber’s method(p.3.2.)Suppose that for the first sample the result is 2,0 %F, for the second – 5,9%F.Second – determine the milk density, using aerometer (p.3.1.)Suppose that the results are 1,0316 for the first sample and 1,0274for the secondThird – Calculate the SNF content using the formula (p.3.2.3.1.B)0,075∗2,0+ 100−100/1,0316SNF == 8,50%0,3780,075∗5,9+ 100−100/1,0274SNF == 8,23%0,378Fourth – determine the lactose content by the formula (p.3.2.3.2.А)Lact. = SNF * 0,55 = 8.50 * 0.55 = 4.67 %Lact. = SNF * 0,55 = 8.23 * 0.55 = 4.53 %Fifth – determine the salts content by formula (p.3.2.3.3.А /Salts = SNF * 0,083 = 8.50 * 0.083 = 0.71 %Salts = SNF * 0,083 = 8.23 * 0.083 = 0.68 %Sixth – determine the total protein content by formula (p.3.2.3.4.А)Proteins = SNF * 0,367 = 8.50 * 0.367 = 3.12 %Proteins = SNF * 0,367 = 8.23 * 0.367 = 3.02 %So, when calibrating the milk analyser we’ll use samples with the followingparameters:Operation manual 69/98

Ultrasonic milk analyzerI Ist sample(low fat)II nd sample(high fat)milk fat 2,00 5,90SNF 8,50 8,23density 1,0316 1,0274lactose 4,67 4,53salts 0,71 0,68proteins 3,12 3,025.2. For sheep milkDetermination of fat content – Gerber’s method, described in Methods p. 3.4.Density determination – using aerometer, described in Methods p. 3.3.SNF determination – by formula – p. 3.2.3.1.BDetermination of Lactose content – by formula – p. 3.2.3.2.АDetermination of solids/salts content – by formula – p. 3.2.3.3.АTotal protein content determination – by formula – p. 3.2.3.4.АExample: Determination of the quality parameters for two samples sheepmilk (low fat and high fat), obtained and prepared according p. 2.3.1 and2.4.1.First – determine the fat content in the samples, using the Gerber’s method(p.3.2.)Suppose that for the first sample the result is 5,6 %М, for the second – 9,8%М.Second – determine the milk density, using aerometer (p.3.1.)Suppose that the results are 1,0352 for the first sample and 1,0300for the secondThird – Calculate the SNF content using the formula (p.3.2.3.1.B)0,075∗5,6+ 100−100/1,0352SNF == 10,11%0,3780,075∗9,8+ 100−100/1,0300SNF == 9,65%0,378Fourth – determine the lactose content by the formula (p.3.2.3.2.А)Lact. = SNF * 0,45 = 10.11 * 0.45 = 4.55 %Lact. = SNF * 0,45 = 9.65 * 0.45 = 4.34 %Fifth – determine the solids content by formula (p.3.2.3.3.А /Salts = SNF * 0,075 = 10.11 * 0.075 = 0.76 %Salts. = SNF * 0,075 = 9.65 * 0.075 = 0.72 %Operation manual 70/98

Ultrasonic milk analyzerSixth – determine the total protein content by formula (p.3.2.3.4.А)Proteins = SNF * 0,475 = 10.11 * 0.475 = 4.80 %Proteins = SNF * 0,475 = 9.65 * 0,475 = 4.58 %So, when calibrating the milk analyser we’ll use samples with the followingparameters:I Ist sample(low fat)II nd sample(high fat)milk fat 5,60 9,80SNF 10,11 9,65density 1,0352 1,0300lactose 4,55 4, 34salts 0,76 0,72proteins 4,80 4,585.3. For wheat, buttermilk and creamDetermination of fat content – Gerber’s method, described in Methods p. 3.4.Density determination – using aerometer, described in Methods p. 3.3.SNF determination – using drying - p. 3.3. and formula – p. 3.2.3.1.АOperation manual 71/98

Ultrasonic milk analyzerAPPENDIX 5: EASY CALIBRATION OF THE MILK ANALYSERBY CALCULATING THE BASIC PARAMETERS VIA FORMULASDETERMINATION OF THE BASIC PARAMETERS IN THE MILK SAMPLEBY USING FORMULAS IS NOT AS PRECISE AS USING THE ARBITRARYMETHODS, BUT IS SUITABLE FOR USAGE IN FIELD WORK.5.1. Determination some of the parameters by formulasThere is dependence between the different parameters in milk and itsdensity, which may be expressed with mathematical equation. On this basedifferent formula, tested and confirmed by the classical laboratory methodsfor analyses, are developed. We recommend the following:5.2. SNF determination.For determination of SNF the correlation dependence exists between themilk’s density, fat and SNF in the milk. When the density and the fat areknown, the SNF can be calculated.There are several formulas with different applicability.А/ When the salts and fat are knownSNF is calculated by subtracting the fat percentage from the salts.SNF = Salts – F (%)WhereSalts – salts in (%),F – fat content in (%),This formula is used for determination of SNF in whey, buttermilk, and cream.B/ Known quantity of fat and density (most commonly used method whenmaximum accuracy is needed).We recommend the following formula:0,075∗F%+ 100−100/densitySNF =0,378This is a universal formula and actual for milk of almost all kind of cows andsheep all over the world.Operation manual 72/98

Ultrasonic milk analyzer5.3. Determination of lactose contentWe recommend the following formulas:А/ for cow milkLact. = SNF * 0,55 (% )WhereSNF – content of SNF in percentages (%),0,55 – constant coefficient.B/ for sheep milkLact. = SNF* 0,45 (% )WhereSNF –solids-non-fat content in percentages (%),0,45 – constant coefficient.This is an actual coefficient for sheep breeds on the territory of the BalkanPeninsula.5.4. Determination of salts contentWe recommend using the following formulas:А/ for cow milkSalts = SNF* 0,083 (% )WhereSNF – solids-non-fat content in percentages (%),0,083 – constant coefficient.B/ for sheep milkSalts = SNF * 0,075 (% )WhereSNF – solids-non-fat content n percentages (%),0,075 – constant coefficient.Operation manual 73/98

Ultrasonic milk analyzerThis is an actual coefficient for sheep breeds on the territory of the BalkanPeninsula.5.5. Determination of total proteins contentWe recommend using the following formulas:А/ for cow milkProtein = SNF * 0,367 (% )WhereSNF - solids-non-fat content in percentages (%),0,367 – constant coefficient.B/ for sheep milkProtein = SNF * 0,475 (% )WhereSNF – solids-non-fat content in percentages (%),0,475 - constant coefficient.This is an actual coefficient for sheep breeds on the territory of the BalkanPeninsula.Operation manual 74/98

Ultrasonic milk analyzerAPPENDIX 6 FREEZING POINT DETERMINATION1. Methods for determination.The milk analyzer determines the freezing point of each sample and thequantity of added water. The milk analyser does not measure the freezingpoint, but calculates it from the components it depends on. The basiccomponents in the milk are water, solids, lactose, FAT, proteins, minerals(salts) and acids. The freezing point depends only on the diluted in the milkcomponents and quantity of the solvent (in the milk it is water). The ultrasonictechnology allows direct measurement of FAT, proteins, lactose + salts (thesoluble components, only influencing the freezing point), and the quantity ofthe solvent in % is determined by 100 % – total solids %, total solids = lactose% + FAT % + proteins % + salts % + acids %.Without understanding the meaning of the freezing point – determined orshown from the milk analyzer added water result easily may lead to a mistakefor the value of this parameter.2. The basic freezing point.Milk freezes at lower temperature than water. The average freezing point ofthe raw milk in the most regions is at about -0,540°С. The average readingfor your region is called “basic” freezing point.The freezing point of milk is a “physiological constant”. This does not meanthat it will not vary. In fact feed, breed, season, time of lactation, climate,whether the sample is taken at the beginning, middle or end of lactation – allthese factors will have an effect on the freezing point of the individual sample.This means that there is an average value of all these numbers. The moresamples used in obtaining this average, the more reliable it is as a base. Orthe basic freezing point is an average of freezing points of milk, taken frommany cows. When a laboratory checks a producer, it is only comparing theaverage of the producer’s cows against a larger area average.The Health authorities establish the basic freezing point or agriculturedepartments in some regions, sometimes by universities, separate dairyproducers, or their associations. Frequently, tolerances have beenestablished on top of a basic freezing point to allow some variations in themilk as well as device or operator variations.Without mentioning the basic freezing point, the Association of OfficialAnalytical Chemists now recommends an upper limit freezing point at -0,525°C (2,326 standard deviations above the most recently determinedNorth American average of –0,5404°C), below which there will be at 95%Operation manual 75/98

Ultrasonic milk analyzerconfidence that will show 99% of all freezing point determinations onunwatered milk:“if the freezing point is –0,525°C or below, milk may be presumed to be freeof water or may be confirmed as water free by tests, specified below. If thefreezing point is above –0,525°C, milk will be designated as “presumptiveadded water” and will be confirmed as added water or added water free bytests specified below. Evaluate extreme daily fluctuations in the freezing pointof herd, pooled herd, or processed milk for presence of added water”.“Presumed added water”, as described above, must be “confirmed” by meansof tests on authentic milk samples obtained as specified in the АОАСMETHODS.After determination the freezing point of your sample via the milk analyzer,the added water is calculated using the following formula:AddedWater =FrPointBaseFrPoint− FrPointBaseCalc∗100[%]Where:FrPointBase is the basic freezing pointFrPointCalc is measured freezing pointNote:If the freezing point is not correctly determined, the result for the added wateris not valid. In this case results for FrPoint and AddWater are not shown onthe display and on the printout from the printer. If the density of the measuredsample is 0, the result for AddWater is not valid and is also not shown on thedisplay and the printouts.Sample:First variantIf you’ve entered for milk analyzer basic freezing point -0.520°C (accordingarticle 5.9 of the EU Milk Hygiene Directive 92/46/ЕЕС), measured freezingpoint –0.540°C, using the above pointed formula you’ll receive –3,8%.Because it is not possible the added water to be negative value, the milkanalyzer indicates 0% added water. The reason for this is the tolerance in thebasic freezing point, reasons for which are described below.If in the same milk we add 3,8% water, and the basic freezing point is thesame, the milk analyzer will measure freezing point –0.520°C, and willindicate again 0% added water.Second variantOperation manual 76/98

Ultrasonic milk analyzerIf you’ve entered for the device basic freezing point –0.540°C, measuredfreezing point –0.540°C, the milk analyzer will indicate 0%. When you add3,8% water, the device will indicate 3,8%-added water.From the above mentioned follows that it is very important to enter correctbasic freezing point in the device.The device’s results for added water may give information about doubtof added water in the milk and the exact value of this added water maybe determined after a “cowshed sample” is taken and the result for thefreezing point, measured by the milk analyzer of the “cowshed sample”is entered as basic freezing point in the formula for calculation of addedwater.Then the result from this formula will give us the absolute value of the addedwater for the corresponding milk supplier.Operation manual 77/98

Ultrasonic milk analyzerAPPENDIX 7 PH MEASURING1. General informationPH probe is a unit, measuring the solution acidity or alkalinity degree. It ismeasured on scale of 0 to 14. The term pH is derived from "p", themathematical symbol for the negative logarithm, and "H", the chemicalsymbol of Hydrogen. The formal definition of pH is the negative logarithm ofthe Hydrogen ion activity.2. pH ElectrodeFor pH measurement the milk analyzer needs a combination electrode,compatible with most pH electrodes that have BNC connectors and zeropotential (the pH where the mill volt output of the electrode equals 0) near 7pH.2.1. Electrode partThe electrode is the most important part of the pH measurement. Theelectrode glass membrane is fragile and must be handled with care. Toprotect the glass membrane and to maintain activation, a protective rubbercap containing a suitable storage solution covers the glass membrane.2.2. Electrode care & Electrode maintenancepH Electrodes are susceptible to dirt and contamination and need to be cleanregularly depending on the extent and condition of use. At no time should onetouch or rub the glass bulb as this causes the build-up of electrostatic charge.2.3. StorageFor best results, always keep the pH bulb wet. An optimal storage solution forcombination electrode is pH 4 buffer with 225 grams of KCl per liter. Tablesalt, NaCl, can be used if KCl is not really available. Other pH buffers or tapwater are also acceptable storage media, but avoid storage in de-ionizedwater. The protective rubber cap filled with the buffer solution provides idealstorage for long periods.2.4. After UseAfter measurement is completed, follow the sequence below for storage.- Wash the electrode and reference junction in de-ionized water.- Close the refilling hole by returning its rubber sleeve or stopper cap.(Necessary for only refillable electrode).- Store the electrode as mentioned above (see section Storage).Operation manual 78/98

Ultrasonic milk analyzer2.5. Electrolyte Replacement (for refillable electrode only).The reference electrolyte needs to be refilled when the electrode has beenused for a long period, or when the internal electrolyte has dried up. Toaccomplish this, follow the procedure described below.- Remove the protective rubber cap or sleeve;- Remove the protective rubber sleeve to expose the filling port of theelectrode;- Remove the old reference electrolyte with a syringe;- Fill the new reference electrolyte.2.6. New electrolyte preparation:- Open the KCl container;- Add in de-ionized water until it reaches the level of 20 ml;- Close the container and shake it to dissolve the KCl;- Add in fresh electrolyte until it reaches the level of the refilling port. Thereference electrolyte used should be 3M(Mol) KCl;- Replace the rubber sleeve.2.7. Re-use the electrode.- Rinse the liquid junction with de-ionized water.If these steps fail to restore normal electrode response, you may attempt torejuvenate it (See: Electrode Rejuvenation).2.8. Electrode cleaningElectrodes which are mechanically intact can often be restored to normalperformance by one or combination of the following procedures.- Salt deposits:Dissolve the deposit by immersing the electrode in tap water for ten to fifteenminutes. Then thoroughly rinse with de-ionized water. Wash the electrode pHbulb in a little detergent and water. Rinse electrode tip in with de-ionizedwater.- Oil/Grease films:Wash electrode pH bulb in a little detergent and water. Rinse electrode tipwith de-ionized water.- Clogged Reference Junction:pH electrodes have junction, which allows the internal fill solution of themeasuring electrode to leak out into the solution being measured. TheOperation manual 79/98

Ultrasonic milk analyzerjunction can become clogged by contamination in the solution. If a cloggedjunction is suspected it is best to clear the junction.Heat up the diluted KCl solution to 60-80°C. Place the sensing part of the pHelectrode into the heated KCl solution for approximately 10 minutes. Allow theelectrode to cool while immersed in some unheated KCl solution.- Protein DepositsPrepare 1% pepsin solution in 0.1 M HCI. Allow the electrode to stand in thissolution for five to ten minutes. Rinse the electrode with de-ionized water.2.9. Electrode activationGenerally, if the procedure of storage and maintenance had been closelyfollowed, the electrode canbe used immediately. However, should the electrode response becomesluggish, it may be possible that the bulb has dehydrated.The bulb can be dehydrated by immersing the electrode in an ideal storagesolution (e.g. buffer pH 4 solution) for 1-2 hours. If this fails, the electrodemay require re-activation. If the above procedure does not reactivate theelectrode to acceptable status, try rejuvenation the electrode by following theprocedure outlined below.2.10. Rejuvenation ProcedureDip and stir the electrode in freon or alcohol for 5 minutes.Leave the electrode in tap water for 15 minutes.Dip and stir the electrode in concentrated acid (HCI, H 2 S 4 ) for 5 minutes.Leave the electrode in tap water for 15 minutes.Dip and stir in strong base (NaOH) for 5 minutes.Leave the electrode in tap water for 15 minutes.Test with standard calibration solution.Finally, test with standard calibration buffer solution to see if the electrodeyields acceptable results. You may repeat again for better response(maximum 3 times). If the response does not improve, then the electrode hascompleted its useful life. Replace with a new electrode.2.11. Electrode LifespanpH electrodes have a finite lifespan due to their inherent properties. How longa pH electrode will last will depend on how it is cared and the solution it isused to measure. Even if an electrode is not used it still ages. Electrodedemise can usually be characterized by a sluggish response, erratic readingsor a reading, which will not change. When this occurs an electrode can nolonger be calibrated. pH electrodes are fragile and have a limited lifespan.How long an electrode will last is determined by how well is maintained andthe pH application. The harsher the system, the shorter the lifespan. For thisOperation manual 80/98

Ultrasonic milk analyzerreason it is always a good idea to have a back-up electrode on hand to avoidany system down time.3. Buffer SolutionsBuffers are solutions that have constant pH values and the ability to resistchanges in that pH level. They are used to calibrate pH measurementsystem.PH buffer solution description ( Pharmacopoeia standard)Use only this types standard buffers for calibration!Description pH 7.00±0,01/20ºC pH 4.00±0,01/20ºCCompositionPotassium dihydrogen Borax, Sodiumphosphate, Di-sodium hydroxide solutionhydrogen phosphateTemperatureparameters4. pH Electrode Calibration10ºC - 7.0625ºC - 6.9920ºC - 7.0030ºC - 6.9840ºC - 6.9550ºC - 6.9110ºC - 4.0025ºC - 4.0020ºC - 4.0030ºC - 4.0040ºC - 4.0050ºC - 4.05pH Electrodes are like batteries; they run down with time and use. As anelectrode ages, its glass changes resistance. For this reason, electrodesneed to be calibrated on a regular basis. Calibration in pH buffer solutioncorrects for this change.Calibration is an important part of electrode maintenance. This assures notonly that the electrode is behaving properly but that the system is operatingcorrectly.Usually pH meters require calibration at 3 specific pH values. One calibrationis usually performed at pH 7, second and third are typically performed at pH 4and pH 10.It is best to select a buffer as close as possible to the actual pH value of thesample to be measured. Use standard calibration buffers that thetemperature and the sample solution are the same.Use the operation manual for the corresponding pH meter.Operation manual 81/98

Ultrasonic milk analyzerFor Sensorex pH electrodes, originally supplied with Lactoscan read thefollowing information:Temperature compensationsThe output of pH electrodes varies with temperature in manner, predicted bytheory. When needed, Sensorex can supply electrode holders with build-inautomatic temperature compensators. The need of automatic compensationdepends on the temperature variation, the pH value being measured. At pHof about 7 there is no error due to temperature and, of course, at a constanttemperature there is no error. As shown in the following table, the pH errordue to temperature is a function of both the temperature and the pH valuebeing measured. At a pH of about 7 there is no error due to temperature and,of course, at a constant temperature there is no error. The more thetemperature changes from the ambient calibration temperature and the morethe pH departs from 7 the greater is the pH error.pH temperature error table°C pH2 3 4 5 6 7 8 9 10 11 125 .30 .24 .18 .12 .06 0 .06 .12 .18 .24 .3015 .15 .12 .09 .06 .03 0 .03 .06 .09 .12 .1525 0 0 0 0 0 0 0 0 0 035 .15 .12 .09 .06 .03 0 .03 .06 .09 .12 .1545 .30 .24 .18 .12 .06 0 .06 .12 .18 .24 .3055 .45 .36 .27 .18 .09 0 .09 .18 .27 .36 .4565 .60 .48 .36 .24 .12 0 .12 .24 .36 .48 .6075 .75 .60 .45 .30 .15 0 .15 .30 .45 .60 .7585 .90 .72 .54 .36 .18 0 .18 .36 .54 .72 .900 pH Error Range Less than .1 pH Error Range5. PH helpful hintsFor greatest accuracy in pH measurement, follow these guidelines:Use the same technique to measure samples, which was used for calibration.Be consistent with stirring rates, times and conditions.Calibrate with buffers, which are close in temperature to that of the sample.Calibrate the pH electrode regularly, e.g. once an hour for accuracy to within0.01 pH, or once a day for accuracy to within 0.1 pH.Use fresh buffers for calibrations. Avoid contamination of the stock buffersolution and do not use it beyond the expiry date.Keep all connections dry.Operation manual 82/98

Ultrasonic milk analyzerImmerse the electrode far enough into the solution to insure the referencejunction is below the surface.Allow adequate time for the electrode to stabilize in standards and samplesbefore taking a reading.Clean the electrode periodically. Allow more time for aged electrodes.Do not use the pH electrode in solutions of fluoride ion at low pH. This willetch the glass membrane.Sulphide vapors can permeate the electrode wick and contaminate thereference element. Minimize contact in such environments and change thereference electrolyte frequently.6. PH measuring.Measuring pH is an additional feature of the analyzer and is optional.Remove the protective rubber cap of the pH electrode. Take care to handle itappropriate in order not to be damaged. Use de-ionized or distilled water torinse the electrode before usage. Fill in the sample holder with milk, put it inthe recess of the analyzer and dip the pH electrode into the milk sample,ensuring complete dip of the electrode in the sample. Stir gently forhomogenization of the sample.Measuring can be done in two modes:Off line by starting the menu pH & Co Meter | Measuring, when theanalyzer works only as a pH meter.On line automatic pH measuring, when measuring the rest of the sample’sparameters.After starting the menu pH & Co Meter the following message appears onthe display:pH CalibrationpH MeasuringpH En/DisablepH U Display-------------------------pH TestCo Meter CalibrCo Meter TestCo Meter En/Dis-------------------------ExitOperation manual 83/98

Ultrasonic milk analyzer7. pH Calibration.Serve for pH meter’s calibration. For this purpose 2 sample buffers are used,shown on the display as Low buffer (for example 3.00 pH) and High buffer(for example 7.00 pH). Follow the procedure:1. Start the Calibration menu.2. Put the probe in the Low buffer.3. Using the analyzer’s buttons enter the exact buffer value. The following isshown on the display:pH CalibrPut Izopot buffBuf=xx.xxx4. The operator has to enter the buffer’s value, when the probe is in itsisopotential point.After that the display shows:pH CalibrPut Izopot buffBuf=xx.xxxV=x.xxxV SetWhere x.xxxxV is the measured in the probe voltage.5. Press the button Set when the readings stop moving.6. Repeat the procedure with the Next buffer. The following messageappears on the display:pH Calibr OKWhich shows that the calibration procedure was completed successfully. Thecalibrated device is ready for making measurements.7. The device automatically passes in mode pH measuring.8. Check the correctness of the calibration by measuring buffer solution 7.00.8. pH Measuring.Operation manual 84/98

Ultrasonic milk analyzerEntering this menu means that you start measurement of pH in off line, i.e.the analyzer works only as a pH meter. The operator has to put the probe inthe sample. The following message is shown on the display:pH measuringx.xxxVy.yy pHExitx.xxx – measured in the probe voltagey.yyy – measured pH of the sampleBy pressing the button Exit, the operator may enter the program and to passto upper menu.9. pH En/Disable.Enables or disables the pH measurement during the normal work of theanalyzer - On line. After staring it, the following message appears on thedisplay:pH MeasuringXXXNo OK YesWhere XXX is the current state of the working mode. By pressing the buttonsunder each of the inscriptions it may be changed. Yes – means that duringthe analyzers normal work the pH will be measured together with the rest ofthe parameters. No – means that the pH measurement will not take place.10. pH U Display.Enables or Disables displaying the measured voltage of the pH probe duringpH measurement. After starting it the display shows the following:PHUDisplayXXXNo OK YesOperation manual 85/98

Ultrasonic milk analyzerWhere XXX is the current state of the displayed mode. By pressing thebuttons below the corresponding inscription it may be changed. Yes – meansthat the voltage of the probe will be shown. No – it will not be shown. It isvalid for the two measuring modes.11. pH testTests the measuring system in production conditions.Operation manual 86/98

Ultrasonic milk analyzerAPPENDIX 8 CONDUCTIVITY MEASURING1. Method of determination.Conductivity (or Electrolytic Conductivity) is defined as the ability of asubstance to conduct electrical current. It is the reciprocal of the resistance.In a healthy animal*, the mean value of electric conductivity is:Milk typeCow milkSheep milkBuffaloConductivity valuesbetween 4 to 6 mS/cm (18°C);between 3 to 5 mS/cm (18°C);between 2,5 to 5 mS/cm (18°C);*These values depend on the geographical region, the breed and on otherfactors.Milk conductivity changes on the concentration of ions in the milk:Added water, sugar,proteins, insolublesolidsAdded saltsSignificantly extremevalue (6,5 - 13,00Decrease the ion's concentration. Milk conductivitydecreases.Increase the ion's concentration. Milk conductivityincreases. Increase the ion's concentration. Milkconductivity increases. Often the milk is falsifiedby adding salt: towards milk with goodcharacteristics: fat 4%, SNF 8,8, conductivity 4,5are added salt and water. Then the results arechanged to 3,2 and 8,8, conductivity 10. In otherwords adding water regulates the increased valueof SNF and density till normal (within theboundaries/parameters) and even the fat isnormal. By the values of these parameters may bedetermined if the sample is falsified, but the onlycharacteristic, proving this is conductivity, which isout of boundaries nevertheless added water. Butbe careful, as the falsification is not the onlypossible reason for conductivity increasing. Theother possibility is mastitis that’s why werecommend using another (chemical) method forchecking it.Should indicate the development of mastitis.Infections damage the tissue of the udder. ThisOperation manual 87/98

Ultrasonic milk analyzermS/cm (18°C)allows sodium and chlorine ions from the blood tobe released into the milk. The concentration ofions in the milk is thereby raised, and it can moreeasily conduct an electrical current - theconductivity of the milk increases.Milk conductivity can be used as tests for degree of water evaporation incondense milk production.Milk conductivity change notifies of powder (dry) milk solution rate.2. Conductivity measurementConductivity measurement is additional possibility of the analyser and isdelivered on customers request/3. Co Meter CalibrServes for conductivity measuring system calibration. Clean the analyzerbefore starting conductivity measurement. (see p. 4.1). You need a standardbuffer with conductivity 5.02[mS/cm] (you may order it for delivery togetherwith the analyser), with temperature 18 o С. After starting this mode, theanalyzer makes preparation for measurement and when it is ready, thefollowing message is displayed:Co Meter CalPut 5.02 buffand press Enterto startThe operator has to put the buffer and to start the measurement. Thefollowing message appears on the display:MeasurementstartedWait pleaseThe buffers' temperature is indicated during measurement. After finishing themeasurement the following message appears on the display:Operation manual 88/98

Ultrasonic milk analyzerCo Pass 1/5=xxxxPut new sampleand press Enterto startWhere xxxx is the result from the first calibration measurement. The operatorhave to put a new buffer, N.B. do not use one and the same buffer more thanonce! Then start the next measurement. This procedure has to be repeated 5times. At the end the following message appears on the display:Cond MeterCalibr= xxxxSwitch Off/OnNow the operator has to switch off the power supply of the analyzer. Afterswitching it on again, the analyser has to be cleaned again with water, whichends the calibration of the conductivity measurement system calibration.Note:Another possibility for calibration of analyzer’s conductivity measurementfunction.You need conductivity meter. First measure milk with normal acidity withconductivity meter and use it as sample for calibrating the analysersconductivity measurement function.4. Co Meter Test.Serves for testing the working mode of the milk's sample conductivitymeasurement system. It is used in the production conditions. After this menuis chosen, the analyser executes the procedure for sample's measurementand the display shows the data, used for obtaining the samples conductivity.Co Meter TestCoADC= xxxxPower Off - Stop5. Co Meter En/Dis.Enables or disables the conductivity measurement system. The followingmessage appears on the display:Operation manual 89/98

Ultrasonic milk analyzerCond MeasuringYesNoYesOK6.Corrections in conductivity measurementIt is done by starting the menu Corrections -> Cond measure. You have thepossibility to increase/decrease the measured conductivity value from – 1.00till +1.00, with step 0.01. After starting this function the display shows thefollowing:Con Meter-1.0=1.0Co Corr=+0.00Edit – Up/DownThe cursor is positioned below the +. By using buttons Up/Down, theoperator has the possibility to change the value (number). By pressing thebutton Enter, the operator confirms the chosen value and moves to the nextposition for editing it. After the last position is edited, if the correction value iswithin allowed boundaries, the following is displayed: Co Corr Saved, whichmeans, that the correction is entered and saved. On the contrary – it returnsat the beginning and expects valid correction.7. Conductivity calibration buffer preparationIn order a standard buffer for conductivity measuring to be prepared followthe instruction below:1. Take the packet with the powder buffer.2. Carefully shake the packet in order to gather the powder at the bottom.3. Cut one end of the packet.4. Empty its content in a measuring mug with 1 l volume, paying attentionall its content to be emptied.Operation manual 90/98

Ultrasonic milk analyzerFor standard buffer: 5,02 ms – 3,556 г5. Add 600-700 ml distilled water, which was preliminarily deaerated invacuum dryer or boiled and then cooled down to 20 ˚С.6. Shake the mug till the powder is fully dissolved.7. Add distilled water to the mark.Operation manual 91/98

Ultrasonic milk analyzerContents:1. FUNCTION .............................................................................................................................................................62. TECHNICAL PARAMETERS ...................................................................................................................................72.1. WORKING MODES CHARACTERISTICS: ........................................................................................................72.1.1. MEASUREMENT MODE MILK / DAIRY PRODUCT – FIRST TYPE ................................................................................72.1.2. MEASUREMENT MODE MILK / DAIRY PRODUCT – SECOND TYPE ............................................................................72.1.3. MEASUREMENT MODE MILK / DAIRY PRODUCT – THIRD TYPE ...............................................................................72.1.4. CLEANING.............................................................................................................................................................72.2. MEASURING RANGE:............................................................................................................................................82.3. MAXIMUM PERMISSIBLE ABSOLUTE ERROR: ............................................................................................82.4 CORRECT AMBIENT CONDITIONS: ..................................................................................................................92.5. DIMENSIONS: ..........................................................................................................................................................92.6. CONTINUOUS WORKING TIME:........................................................................................................................92.7 MILK SAMPLE VOLUME PER ONE MEASUREMENT:................................................................................10FIG. 3 PRINCIPLE WORKING SCHEME.............................................................................................................................12FIG. 4 PERIPHERALS CONNECTION .......................................................................................................................13FIG. 5 CABLE DESCRIPTION .................................................................................................................................143. QUALIFICATION OF RAW MILK, THERMALLY TREATED MILK, OTHER DAIRY PRODUCTS ANDDERIVATIVES ..............................................................................................................................................................153.1. TAKING SAMPLES AND PREPARATION FOR ANALYSES........................................................................153.2. MAKING THE MEASUREMENT........................................................................................................................153.2.1. PREPARING THE ANALYZER FOR WORKING MODE ...............................................................................................153.2.2. MAKING ANALYSES ............................................................................................................................................163.2.3. DISPLAYING THE RESULTS ..................................................................................................................................174. CLEANING THE ANALYZER................................................................................................................................194.1. PERIODICALLY CLEANING (RINSING) THE ANALYZER ........................................................................194.1.1. PERIODICAL CLEANING FREQUENCY. ..................................................................................................................194.1.2. MAKING THE RINSING .........................................................................................................................................204.2. COMPLETE CLEANING......................................................................................................................................204.2.1. COMPLETE CLEANING FREQUENCY .....................................................................................................................204.2.2. CLEANING...........................................................................................................................................................20FIG. 6 LABELS FOR THE CLEANING CHEMICALS.............................................................................................................214.3. PERISTALTIC PUMP SERVICE...................................................................................................................................22FIG.7 PERISTALTIC PUMP ..............................................................................................................................................225. POSSIBLE MALFUNCTIONS AND ERROR MESSAGES, TROUBLESHOOTING .....................................225. POSSIBLE MALFUNCTIONS AND ERROR MESSAGES, TROUBLESHOOTING .....................................236. MAKING CORRECTIONS AND RECALLIBRATION OF THE DEVICE.......................................................256.1. TAKING SAMPLES AND PREPARATION OF SAMPLES FOR CHECKING THE ACCURRACY OFTHE MILK ANALYSER, MAKING CORRECTIONS AND RECALIBRATION ................................................256.2. DETERMINATION THE TYPE OF THE DISCREPANCY: ............................................................................256.2.1. MAKING MEASUREMENTS...................................................................................................................................25Operation manual 92/98

Ultrasonic milk analyzer6.2.2. ANALYSING THE MEASUREMENT RESULTS..........................................................................................................256.3. MAKING CORRECTIONS ...................................................................................................................................266.3.1. POSSIBLE CORRECTIONS, LIMITS AND CHANGING STEPS......................................................................................266.3.2. PREPARING THE ANALYZER FOR MODE CORRECTIONS ........................................................................................276.3.3. MAKING CORRECTION.........................................................................................................................................276.4. RECALIBRATING THE MILK ANALYSER.....................................................................................................296.4.1. RUNNING THE ANALYSER IN MODE RECALIBRATE ..............................................................................................296.4.2. MAKING RECALIBRATION ...................................................................................................................................307. STARTING THE DEVICE IN A SERVICE TEST/SETUP OPERATIONAL MODE. MENUSDESIGNATION..............................................................................................................................................................357.1. STARTING THE DEVICE IN A SERVICE TEST/SETUP OPERATIONAL MODE....................................357.2. MENUS FUNCTION: .............................................................................................................................................367.2.1. SPECIAL MODES. .................................................................................................................................................367.2.2. CORRECTIONS.....................................................................................................................................................367.2.3. SETTINGS. ...........................................................................................................................................................377.2.4. TESTS..................................................................................................................................................................427.2.6. EXIT....................................................................................................................................................................437.2.7. MILK ANALYSERS’ SETUP MENU STRUCTURE......................................................................................................438. ADDITIONAL POSSIBILITIES OF THE ANALYZER .......................................................................................478.1. CONNECTING TO 12 V DC POWER SUPPLY.................................................................................................478.2. CONNECTING TO IBM PC..................................................................................................................................478.3. CONNECTING A PRINTER (OPTION)..............................................................................................................478.4. CONNECTING AND WORKING WITH EXTERNAL KEYPAD (OPTION). ...............................................478.5. EMBEDDED REAL TIME CLOCK (OPTION). ...............................................................................................................49APPENDICES .............................................................................................................................................................50APPENDIX 1 METHODS .............................................................................................................................................501. DETERMINATION OF MILK'S DENSITY...........................................................................................................501.1. GENERAL ...............................................................................................................................................................501.2. SAMPLING AND PREPARATION FOR ANALYSES ......................................................................................501.3. BASIC PRINCIPLES..............................................................................................................................................501.4. NECESSARY DEVICES AND REAGENTS........................................................................................................501.5. MAKING THE DETERMINATION: ...................................................................................................................501.6. RECALCULATING THE VALUES ACCORDING LACTO-DENSITY-METER AT 20 OС.......................512. DETERMINATION OF FAT CONTENT IN THE MILK AND MILK DERIVATIVES. .................................512.1. GENERAL ...............................................................................................................................................................512.2. SAMPLING..............................................................................................................................................................512.3. BASIC PRINCIPLES..............................................................................................................................................512.4. NECESSARY DEVICES AND REAGENTS........................................................................................................51Operation manual93/98

Ultrasonic milk analyzer2.5. MAKING THE DETERMINATION: ...................................................................................................................522.6. MAKING MEASUREMENT .................................................................................................................................522.7. CALCULATING THE RESULTS.........................................................................................................................522.8. MEASUREMENT ACCURACY ...........................................................................................................................533. DETERMINATION OF WATER CONTENT AND SOLIDS IN THE MILK AND MILK DERIVATIVES..533.1. GENERAL ...............................................................................................................................................................533.2. BASIC PRINCIPLES..............................................................................................................................................533.3. NECESSARY DEVICES AND REAGENTS........................................................................................................533.4. MAKING THE DETERMINATION: ...................................................................................................................543.5. MAKING THE MEASUREMENT........................................................................................................................543.6. CALCULATING THE RESULTS.........................................................................................................................543.7. MEASUREMENT ACCURACY. ..........................................................................................................................544. DETERMINATION OF CASEIN CONTENT IN THE MILK. ............................................................................554.1. GENERAL ...............................................................................................................................................................554.2. SAMPLING..............................................................................................................................................................554.3. BASIC PRINCIPLES..............................................................................................................................................554.4. NECESSARY DEVICES AND REAGENTS........................................................................................................554.5. MAKING THE DETERMINATION: ...................................................................................................................554.6. MAKING THE MEASUREMENT........................................................................................................................554.7. CALCULATIONS...................................................................................................................................................564.8. MEASUREMENT ACCURACY. ..........................................................................................................................575. DETERMINATION OF SALTS IN THE MILK ....................................................................................................575.1. GENERAL ...............................................................................................................................................................575.2. SAMPLING..............................................................................................................................................................575.3. BASIC PRINCIPLES..............................................................................................................................................585.4. NECESSARY DEVICES AND REAGENTS........................................................................................................585.5. MAKING THE DETERMINATION: ...................................................................................................................585.6. CALCULATIONS...................................................................................................................................................585.7. MEASUREMENT ACCURACY ...........................................................................................................................58APPENDIX 2 REPRESENTATIVE SAMPLES FROM MILK AND OTHER MILK DERIVATIVES FORMILK ANALYSER’S CALIBRATION .......................................................................................................................59Operation manual94/98

Ultrasonic milk analyzer1. GENERAL ..................................................................................................................................................................592. NECESSARY QUALITY PARAMETERS VALUES DETERMINATION .................................................................................592.1. LABORATORY METHODS .................................................................................................................................592.1.1. DETERMINATION OF FAT CONTENT .....................................................................................................................592.1.2. MILK DENSITY DETERMINATION .........................................................................................................................602.1.3. DETERMINATION OF TOTAL PROTEINS.................................................................................................................602.1.4. DETERMINATION OF CASEIN CONTENT IN THE MILK............................................................................................612.1.5. DETERMINATION OF SALTS IN MILK. ...................................................................................................................612.1.6. DETERMINATION OF SOLIDS IN MILK...................................................................................................................61EXPRESS METHODS BY USING ANOTHER MILK ANALYSERS.....................................................................61APPENDIX 3 MILK SAMPLING AND PREPARATION OF SAMPLES FOR ANALYSES...............................621. GENERAL ..................................................................................................................................................................622. STIRRING THE MILK AND ITS DERIVATIVES BEFORE SAMPLING .................................................................................623. SAMPLING.................................................................................................................................................................634. SAMPLE PRESERVATION............................................................................................................................................635. PREPARING THE SAMPLES FOR ANALYSES.................................................................................................................63APPENDIX 4 SAMPLING AND PREPARATION OF SAMPLES FOR VERIFICATION THE ACCURACYOF THE MILK ANALYSER, MAKING CORRECTIONS AND RECALIBRATION..........................................651. NECESSARY CONSUMABLES AND DEVICES ................................................................................................................652. GENERAL ..................................................................................................................................................................653. REPRESENTATIVE SAMPLES......................................................................................................................................654. SAMPLES PREPARATION ............................................................................................................................................675. ADVISABLE SCHEME FOR INDEPENDENTLY DETERMINATION THE CONTENT OF DIFFERENT PARAMETERS IN MILK ANDITS DERIVATIVES...........................................................................................................................................................685.1. FOR COW MILK (WHOLE MILK, LOW FAT, SKIMMED MILK) AND UHT MILK...............................695.2. FOR SHEEP MILK.................................................................................................................................................705.3. FOR WHEAT, BUTTERMILK AND CREAM....................................................................................................71APPENDIX 5: EASY CALIBRATION OF THE MILK ANALYSER BY CALCULATING THE BASICPARAMETERS VIA FORMULAS ..............................................................................................................................725.1. DETERMINATION SOME OF THE PARAMETERS BY FORMULAS.........................................................725.2. SNF DETERMINATION. ...........................................................................................................................................725.3. DETERMINATION OF LACTOSE CONTENT ................................................................................................................735.4. DETERMINATION OF SALTS CONTENT.....................................................................................................................735.5. DETERMINATION OF TOTAL PROTEINS CONTENT ....................................................................................................741. METHODS FOR DETERMINATION. ..............................................................................................................................752. THE BASIC FREEZING POINT. .....................................................................................................................................751. GENERAL INFORMATION ...........................................................................................................................................782. PH ELECTRODE.........................................................................................................................................................782.1. ELECTRODE PART ..............................................................................................................................................782.2. ELECTRODE CARE & ELECTRODE MAINTENANCE ................................................................................782.3. STORAGE................................................................................................................................................................782.4. AFTER USE.............................................................................................................................................................782.5. ELECTROLYTE REPLACEMENT (FOR REFILLABLE ELECTRODE ONLY)........................................792.6. NEW ELECTROLYTE PREPARATION:...........................................................................................................792.7. RE-USE THE ELECTRODE. ................................................................................................................................79Operation manual95/98

Ultrasonic milk analyzer2.8. ELECTRODE CLEANING....................................................................................................................................792.9. ELECTRODE ACTIVATION ...............................................................................................................................802.10. REJUVENATION PROCEDURE .......................................................................................................................802.11. ELECTRODE LIFESPAN ...................................................................................................................................803. BUFFER SOLUTIONS ..................................................................................................................................................814. PH ELECTRODE CALIBRATION ..................................................................................................................................815. PH HELPFUL HINTS ...................................................................................................................................................826. PH MEASURING.........................................................................................................................................................837. PH CALIBRATION......................................................................................................................................................848. PH MEASURING. .......................................................................................................................................................849. PH EN/DISABLE. .......................................................................................................................................................8510. PH U DISPLAY. .......................................................................................................................................................8511. PH TEST ..................................................................................................................................................................861. METHOD OF DETERMINATION. ..................................................................................................................................872. CONDUCTIVITY MEASUREMENT......................................................................................................................883. CO METER CALIBR ................................................................................................................................................884. CO METER TEST. ....................................................................................................................................................895. CO METER EN/DIS. .................................................................................................................................................896.CORRECTIONS IN CONDUCTIVITY MEASUREMENT...................................................................................907. CONDUCTIVITY CALIBRATION BUFFER PREPARATION ..........................................................................90Operation manual96/98

Ultrasonic milk analyzerGUARANTEE CARDStandard modelGuarantee period is 1 (one) year after purchasing date.Improper handling, transport and storage will invalidate the guarantee.Guarantee is void if warranty labels are removed.Serial №Date of purchase:Password:Distributor:Signature:Stamp:Operation manual97/98

Ultrasonic milk analyzerGUARANTEE CARDPurchaser:Service report:Serviceentry dateDamageDeliverydateSignatureCovers:MIA-S, software version 50, LCD display, software version 45Operation manual 98/98

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