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Manual Photometer SQ 118 MERCK This manual is divided into three sections, 1. General information Tho first section deals with the funcamental principles and practice related aids for carrying out photometric analyses. Subjects which are important for correct analys's ranging from the preparation of samples through numerous hints for measuring practice and ensuring quaily are also treated 2. Analytical methods tans a collection ofall the an: methods in the Spectroquant ready-to-use test 1 ne measured with the $Q 118 photometer. On a moth sheet, with the help of llustrations, each method is clearly described in an easily understandable fash 3, Operating the SQ 118 photometer Inthe third section, the technical section, a detailed description of the operation of the SQ 118 photometer all its options is given. In addition to easy routine analysis with Spectroquant tests, user generated methods can be programmed and special problems can be soived. As a rule, the user mil not be able te oxhaver al of tho poesibiitlee which the device offers. In this respect the technical section serves more as a reference work, particularly since the user is already supported by the competent quidan display. o given MERCK Se as Ut the dotermiaton principe yaa 112. rndamenta pepe stphatomaiy. 8 Baa 113. Show penton sequence ofthe protometer 18 343 11a. Metoa tet wit measuring range. “a aia iii og Tating samples aa Precing, a4 baton 322 Inorecing te concertaion. 323 Drtorentston ot forma of appearence, a2 Fitrevon. ozs pt coretion aa? aaa 4.8m to inci practi bo {a1 ormoronctor TR 007TR 200 132. Proton pipettes aa 122. gn Me ote reagents aaa 124 Doahg the ressont. aa 138. blonke oa 138 fluence oftemperatie 127 Time capendency. aa 120 calwenagaes dnvcas aa 139. Gonnuereton of tne risus slau ana of amples baa 1.240 Apooabity in sos weter aaa 1.3.11. Measuring high concentrations. 1.3.12 Safety hints . 14 Quality control. i 1.4.1 Measurements at the lower lit measuring rang 14.2 Standard solutions 1.43 System dependent 4.44 Sample dependent influences. 34.13 145 Reducing possibilities of error. 34.14 24 2.2 Spectroquant cell tests - 2.3 Method number... 24 Further information. . : 355 356 CRESS ROL ‘Description of the Instrument... 2114 Installation... 2114 Mains operation 144 Battery operation . 115 115 Cell compartment. Keyboard . 115: Carrying out an analysis. 7 Lot factor. 118 Series determinations Entry of a sample number . 118 119 Entry of a dilution 119 Last result 120 Renewed zero adjustment 120 ‘Overview with all options. 120 Result marking . 122 Calculation of results =. 122 Programming a method - 123 Evaluation with factors. 124 Evaluation with standard solutions. 127 Structure of parameters Description of the function . Printing out results . Displaying results Transferring results to a computer Setting of a consecutive number. Printing out the method list . Printing out the parameter list. . Printing out the function list - To start the formfeed on the printer Setting the result display time. Setting the date, time and languagé ‘Automatic measurement . .. Computer connection. Service functions. Function structure 131 137 ‘Appendix Printer connection . Computer interface Maintenance and care . Error reports ..- Technical data Delivery programme. MERCK (ere 1.1 The Spectroquant analysis system the holo of madern photometry and the related reagents roquires only a few standard operations, As a result isty, the broad spectrum of water analysis can be dealt simple and relable analysis has been made possible. The n economically. The Spectroquant analysis system makes use of reagents is reduced to a minimum. The volume of the it possible for every user to conduct highly sensitive and formulation must merely be enough for the filing of ane cel sonable costiperlormance ratio. Spectroquant anaiyeis using the SQ 118 photometer is ntact with users this system has been developed described carnprehensively in the second section of this of surface. ground and drinking water, cainfall, manual and waste water. However, with the appropriate of samples the analysis of more compiex ch as soil, sold substances and org possibie ss attachments cor quant analysis system. In respect of the pre-treatment of samples, the thermoreactor TR 200 is used for the heating of samples. a ing of 12 COD structed in materials The central element of the Its nighiy develo ogy is optimally istry of the Spectroguant tests, parameters are pre-programmed. The Aa cally developed with a view to the requirements {or usortriendly analysis. This has been achioved by the inclusion of the latest microprocessing technology in connection with high quality elect ponents, The mavaments requir for narrying oui a termination have been reduced to a minimum, The SQ can be transported in a case with accessories, In this way mobile analysis directly on site, and independent of the ins, is po: only tho ki exact dilution and measurement of the sample volume, Ready-to-use standard solutions guarantee reliable and reproducible results, he results obtained + sorted according to method {algo controla and monitors all of + sorted according to sariiphen the se shotometer. it makes sure, for example, ‘i jomary prin bo cont that the correc fiter is always automatically placed in the ne used. For special tasks data transfer over a stan ight path. interface to a personal computer is possible. In prac Optimization of the classical analysis methods, which in many bilities of he SQ 118 ing with results arose from the German standards for 1d waste minimize sources of error, water testing, led to the development of the Spectroquant losts. The rumorous individual reagents are combined in few liquid concentrates and powdered mixtures. Dos! MERCK 1.1.1 The determination principle The determination principle is concerned with a colour reac: lion of a specific reagent and the contents of the sample. The intensity of colour is a measure of the concentration content substance | ‘specific colour reagent coloured solution l photometry The Spectroguant tests for photometry contain all the reagents necessary for carrying out an analysis. The liquid reagents are measured by counting the drops from a The block diagram of the SQ 118 photometer provides a ‘schematic representation of the important components of the deviea, such as the light path and data processing. dropping bottle, or in the case of larger volumes with the aid of a piston pipette from a bottle with a leakproof altache- ment. Powdered reagents aro measured out with spoons, Which are usually ineorporated in the screw cap of the bottle. In contrast to the customary practice of carrying out all of the sample formulations in a measuring flask, which is brought Up toa constant volume after the colour reaction time has ‘been completed, the Spectraquant system offers the following advantages: + no topping up with distilled water (open system) + minimal effort + high degree of measurement sensitivity + smaller quantities of liquid ‘The principle of photometric determination is concerned with the weakening in ignt which a monochromatic ight bean ‘experiences when passing through a coloured analysis, solution, The concentration ofthe diluted substance can be ascertained from the strength ofthe light absorbtion. The determination process itself is very simple, and the result is displayed digitally at the press of a key. Construction and measuring principle of the SQ 118 photometer stabilization 41) tungsten halogen lamp 2) aperture 1 9) lens 1 4) aperture 2 5) coll 6) aperture 3 Tens 2 8) interference fiter 9) silicon photodiode 6 9 v 1 intensifier analogue digital transformer keyboard processor memory display Ww 1 The determination principle Focussing of the light beams enables the light from the stabi- lized tungsten halogen lamp to pass through apertures and a lens and reach the cell wih the solution to be tested. A part Cf the ight beam is absorbed in the solution depending on the nature of the substance. The Fight which passes through Is received by the interference fier, which in turn only permits Ww Photometry is an optical analysis process. It uses the weakening of alight beam in a coloured solution to determine the concentration of a substance contained inthe test sample, Normal sunlight is descrived as “white light”. tis a mixlure of ight made up of many wavelengths which can be broken down into colour components, Within the visible range the colours of the rainbow are revealed Colour ‘wavelength Inaige 46 408 be 464-500 green 500-578 yeton 578-502 orange 592-020 te 620-780 that part of the ight to pass through, which is sutable for the ‘substance to be determined by photometric analysis. The silicon photodiode transforms this light into electrical current. This is then intensified and converted into measurement data by the digital converter and a microprocessor. 2 Fundamental principles of photometry Incident light light which has passed through The wavelengths of ultra-violet rays (UV) are below 380 nm. Above 780 are the infra-red rays (IR), Both of these rays are invisible to the eye. For photometry a certain wavelength range, as narrow as possible, is used. A tungsten halogen lamp serves as the light source in the SQ 178, It beams the entire ight spectrum without any gaps. Interference filters are used for the selection of a narrow wavelenath range of ca. 10 nm, A green filter, for example, only allows green light to go ‘through, while all other wavelengths are held back. In the $0 118 photometer white light of diferent wavelengths passes through the sample. A weakening of the light, depending on the nature of the substance, occurs in the light ‘which has passed through. In this wavelength range the Tight intensity of the incident light Ig is reduced to the light intensity lof the ight which has passed through the sample, The ratio of the light after passing through the sample solution ‘and the initial light intensity is described as transmission. tet Assimple, easy to use measure for light absorption is absorbance (A) which has the folowing relationship to transmission’ log T ‘The absorbance increases with the concentration of the substance contained in the test solution and the aptical path longth of the cell. The correlation between these sizes is described by the Lambert Beor Law Lambert ‘eer Law vation absorbance fsbsorbance ceficent oncentation ‘pte! pat nat Pine cal factor ° The absorbance costlicient is a constant specific to the substance and is dependent on the wavelengths used, i.e. itis dependent on the interference filter used. Ifthe optical path length of the cel is kept constant, then transposing the formula produces the simple relationship CHA-F ‘The concentration of the substance contained in the water is obtained by multiplying the measured absorbance by a factor. The factor is dependent on the optical path length of the cell ang the interference fiter. Graphical representation Of this relationship produces a straight line For measuroment with Spactroquant tests all factors F are stored in the SQ 118 photometer. There are, however. ather ‘cases, in which such a simple relationship — as that described above — does not exist. The relationship between the absorbance and the concentration can then be represented by a curve, which can also be programmed in the SO 118 photometer MERCK 8 1.1.3 Short operation sequence of the photometer For users who want fo get a quick averview of the basic ‘operation of tho photometer the short operation sequence wil be introduced here, Carrying [tout can also take the fotm of 2 “dry run" without cells or reagen's. Detailed Information can be found in Section 3 of this manual. This example shows the operator guidance over the two line display. In the first step the desired method is selected using the assigned method number. Next, by pressing the fee) key, a motor automatically positions the filer and, after & few ‘seconds, the requosl "measure blank* appears in the display. The lower line of the display guides with appropriate commentary during the further course of the operation. Selection of method Select biank value Ingert blank Insert test ‘sample ‘Atterinserting the blank cell in the cell compartment the [ll key is pressed and the blank value is stored. The request now is "measure sample“. The cell with tho coloured test sample is placed in the cell compartment. for re-pressing the (13) Key the resuit appears in the display, {An advantage for the user is the fact that after the device has been switched off the method selected remains stored, this means that when the device is switched on again the SQ 118 photometer shows the ‘ast method selected. For the actual determination the result is produced by the three key sequence ese)-—Pa}~- EI). ALUMINIUM AL 8.05 ~ 6.35 ag/I 14825 81 ALUMINIUM AL NEASURE BLANK a1 ALUMINIUM AL NEASURE SAMPLE ALUMINIUM AL, 119 g/l MERCK 1.1.4 Method list with measuring range ~ Reagent tests — No._ Method Cat.No. Meas.Range Unit No. Method Cat.No. Meas.Range_ Unit 201_Aurninium Al 14825 005 - 0.95 _mgh 045_Manganese Mn 44770_0.01 ~ 250 mat (902 Aluminium Al 14825 0.20 — 1.50 _mgf (046 Manganese Mn 1477005 ~~ 10.0 mas (003 Aluminium Al 14825 200-130 mmolim 04” Manganese Mn 4477002 — 48.0 mmole (004 Alumina A 1482574 65.6 _mmolm® 048 Manganoso Mr Ta7I0 9182 mmol 005 Ammonium Ns 14752 0.010 — 0.800 mgh 162 Mercury Hg (0025 — 1.000 mgt (008 Ammonium Ney 16762 0.10 ~3.50 mgt ‘097 _ Ammonium NF W 4752 0.010 - 620 mar 249 _ Nickel wares 0.02 — 200 mg (008 Ammonium Nee N 34752010 ~ 270 mall 60 Nickel N- 14785020 ~ 500 mal (009 Arrenoniur Ney 3476208 44.4 mmolin®_O5t_NckolN 14765 0.4 34.0 mmrolin® (810 _ Arrrnonium NH 147506 = 195 mom? 052 Nickel Ni 1478530” = 850” mmolin® 163 Antimony 5 035 = 800 _mgl 167 Nickel bath Ni 30 120 gf 164 Arsenic As - (0.050 ~ 0.600 ma 053 _Nirate NOs T4773 1.0 250_malh (054 Nitrate NOs 1477350 900m 014 Boron B ____14889 0.050 - 0.600 maf (055 _Nirate NON 4773020 ~ 560 mah (066 _Nirato NOs-N arr. 208 mal 18 _Calckum Ca 14815 5 — 180_mot or_“Haete HO sa 409 mmc 016 Caleium Cad 1aeis 7 224 mah (968 “ivate NOy 147780008 4.45 _ mein? 017 Calcium CaCOs_ 14815 0.13 = 4.00 mmolfin (962 _Nittte NOs 14776 0.020 — 0.600 mgit 920 Chloride CI 14755 1.0 20.0_ mg/l (963 _Nitrite NO 14776 __0.05_— 3.00 _mg fe ennsect jase ose O54 Nite NON "4776 0.910- 0.180 (022 Chiowide CI 1278528 — 554 -mmolim® —-965_Nitite NOs-N 14776 0.02 = 1.00 maf (23 _orioto8 Gi ares 0.28 4.23 maim? 968_NiiteNO 1477604 — 130_memotin® 018 Cherine Cie 14828005 — 1.80” mah 67 Nite NOs 14776 1.0 — 650 menolin® 19. Chtine Gi 01100 mal 171,_Ghlorine Gl 1.50 mgt 147 _Orore Os 14828 0.05 — 1.00 iit 050 — 500ml 179 Orme 0,470.05 — 1.80 mgt 12 “M8 “Chirinesioxde GO, 14828 002 — 1.00_mgh 174 Ozone Os saree 050 —8.00_ ms 169 “Chierinesioxide IO, 14732005 — 1.50 mg {70 Chiinecionids CO, 470060 600 mgf_-«*180_PaladmPd __ a0 = 1.80 mgh__ 24 Crvamium Cr “arse 0010-0600 maf (71 Phosphorus (PHB)P 4848 one — 1.00" mgt ee ee cae ay 912 Phosphor (PMB) vas 0 10 — 500m G6 Shona Oo 3a168 82 LTS mmol 079_Phosphorus PMB) POA 14848 0.06 = 300 mah Gor Ghana ase 20S e074 Phosphorus (PMB) FO 1484803 153 mah 465 Chromumbah GOs 20400 gh ——~=C«7 Phosphorus (PMO)ALOs 14040 0.08 — 2.00 moh a GE TaD eT OTB_Phosorus (PMB) P.O, 14846 0.2 11.5 maf Tee ara 0s Sg «O77 Phosphorus (PMB) PO, V4a® 0532.3 mela ee gas ceo mar «O78 _Phoephorus (PMB) PO, —12e4@ 3 —— v6! mel Spee 10 = $0) mal a8 Phosphons (VM)P taeda 1. = 20.0 -mgh O44 “Copper Cu ‘4767 04 Phosphorus VM)PO, 14842 30 __920_mgt__ oe $0 ee (085 Phosphorus (VM) PO, 1484? 20680 rm GHi"Gyende GN Taio “G00a = Too MeN 9EE_Phosphonus WN) PO, 1404292070 _mmolint 31 Cyanide CN—14800 0.005 — 0500 righ ‘61_Platioum 2 9.10 = 1.50 _ mp 180 Foxmalderyde HCHO 14678 100 — 900ml one Seon ‘fee_030 80 5 094 Siicon SO, 1479402 107 mgt oa0_QusAy __asat_ 09-120 wl 6 Scan Br 1479403 = 285 _mmlin® 090 ~Siioon SiO 7943 = 178 mmoln® 187 Mazencoor 2-200 HZ ag Siver Ag ‘4a01 0.19 = 1.00. ma 138 Hazen coo 10000 HZ a Sir “48a 050 200mg (037 iniazine Ne (ao 003 — 1.00 mah er suiprsio SO, 471 260 mar 038_Hyuiacine Net 14797020 —500 mall 940 SulphideS 14779 0090-0800 mgh (39 Hyorazrne Nets 347o7 06 = 31.2 mmoim? tog SuphigeS tara 025 2400 “Ml 940 “Hyctazine NeHy 14797 6 — 156 mnolin®Yo% “Sulphide 1477006 = 18.1 _mmolin™— 102 Subprige S varr@ 7 —— 121 mmo? +25 _todine colo number 00s —300 Hz +26 Iodine colow number 10-800 FZ 113_tubiaty so =«00 NTU a2 ton Fe “4761 001 = 1.00” mgi 53 hone e761 020 = 2.50 gh 125 Urea 1454405 = 250 maf {34 honFe “7610? —— 100 wrath a35honFe Wisi 36 = 450 mnolir? 109. Zine Zn eg? 005 - 250. moh 122 on WF 023020 - 200 mat 504 Zine zn 1463208 96.2 enol? MERCK 10 1.1.4 Method list with measuring range - Cell tests — No._Method Cat.No._Meas.Range Unit No._Method Gat No. Meas. Range Unit O11 OT AmmoniumNH, 14544 1.0 280 righ 037 _CT Sulphate 60. 1454820 240 malt O12 CT Ammonium NHN E4408 = 217_mgh (098 CT Sulphate 80. $4548__0.2 = 260 molme 013_CTAmmoniymNH, 14844 0.08_— 155 molm® 198 CT Suiphate SO. 74564 190 1000_maf 26 CT Ammonium Ny 1485802 10.0 magi a4 CT Suiphite SO, 149041. 25.0_mgf 327_CTAmmonum NHeN 14558 0.20 ~7.80_mgil 44 CT Surfactants (anionie) 14607 0.05 - 2.00_ mal 32a CT Ammonium NH, 14569. = 100 mgi 23 _CrAmmonum NHN 1486940. - 78.0 mail 162_CTTinsn 14622 0.10 - 250 moll ye3_CT Tota Hardness TH 1456507 220 °o 315_CT. Cadmium o3 14834 0.095 - 1.000 moll 350 CT Chionde Ci 747395125 mall 4105_OT Zine Zn 14565 0.20 - 5.00 moll 306 CT Chromium Ge "4556005 2.00 mot 28 cTCOD, 7454010 150 _mall 230. Absorbance: saonm 0.00 200 & a29_cT.GOD, 74841 100-1800" mal 281_ Absorbance. 05nm 0.00 3.00 A iia _CrcoD 14555800 — 10000 gi 282 Absorbance. a6 nm 0.00 300A 132 _CT COD 40-400 mall 23) Absorbance 495 nm 0.00 300A 14a CT COD 50 = 600 _mgll 284 “Absorbance 25mm 0.00 300A 149 _CTCOD 300” — 3500_mall 235 Absorbance 880mm 0.00 300A 108 CT Copper Go 14559__0.10 — 6.60 mail 236 Absorbance: ‘565.nm 0.00 — 300A 110 CT Cyanice 14561 0.025 0.500. mg/l 257 Absorbance ‘a5am 000 300 A ‘Absorbance {635m 000 3.00 118 CT Ruorige F 14557 0.10 = 1.80_mgi ‘Absorbance ‘650m 000 — 300A 120 CT Formalcehivas 145000. 100 mga ‘Absorbance ‘690m 000 300A ‘Absorbance ‘820nm 000-300 A 184 _CT Hardness Ca 14s05_ 5-140 Transmission ‘adr 00 - 1000 %T 1S _CTHydogenpemide —ar3i__ 20. 200 Transmission 405 nm 00-1000 %T Transmission 446m 0.0 = 1000 &T s0r_CT hon Fe 44849 0.10 — 4.00. mg Transmission 495m 00-1000 %T TTanernssion 525nm 00 = 1000 &T 414 CT Lead Pe 44929 0.40 — 5.00_mga Tanerission ‘550nm 00 = 1000 %T “Transmission 565m 00 — 1000 %1 151 _CT Magnesium Mg éad_—5.0 = 500 mail Transmission ‘sasnm 00 - 1000 xT a5 m0 109 _CT Nickel Ni 910_- 690 moh ‘6am 09) 1059 CT Nirate NO, gh Transmission eaonm 00) (060_CT Nivate NO. mah Transmission e2onm 00 061 CT Nitrate NOs 117 CT Nitrate NOs Ha CT Nivate NON 119 GT Nitrate NOs 748688 mmol 130_CT Nitrate NOs 145632 —— 100 moll a1 CT Nirate NON, 1456308 226 mall 068 CT Nite NOe 14547005 — 2.00 my 068 CT Nite NON 14547 0.020 0.610 mol 70 CT Nie NO; 4547__1.4 43:5 mmol? 140_ CT Nitrogen Nv 1453705 18.0_mgh 168_G1 Oxygen O2 tas 05 120 mot 151 CT Phonols Pro 44851040 — 280 my (079 Cr Phosphowus(PWB)P 14843008 —5.00_mgh (080 _CT Phosphorus (PMB) PO, 1454302 153 _mgh ‘81 er Phosphorus (PMB) FeO, tas 0+ magn (062_CT Phosphorus (PHB) PO. 14543 > imal 142 _CPhosphorus PMB)P_ 14729 1.0 gh 143 CT Phosphorus (PAE 147293 Pag a7 CTPhoeohorus WMP 1464605 mall (056 CT Prosshorus VM) PO, 14546 1.5 ml (089 “CT Phoschows (V)PO, 14546 1.1 — 67.0 mall (080 CT Proschows (vi) PO, 14548 at CT Potassium 62 5.0 500 mal 1 198 _CT Residual Hardness RH 1468 ¥or_CT Residual Hardnoss Ca 14083 16-807 malin gh el rolin® 0.078 - 0.750 *4 060 — 500 gi MERCK 1.2 Preparation of samples From the taking of the sample io the analytical result some fundamental facts must be taker into account. A restriction of the photometric process is that the substance dissolved in the water is only capable of reaction, and will only form the ‘coloured Solan, wine is ie fort of Thee ions Tike ey, CUP Samples frequently contain an abundance of organic compo- ont such as humic acids, complex forming agents, solid substances, or accompanying substances, which interfere with the analytical detection of the substance contained in the water. Complex forming agents, for example, make it possible 1.2.1 Taking samples Every analysis is preceeded by the careful collection of a fepreseniative sample. Here it must be noted thal the Solution to be tested can show varying concentrations In diferent places, at atterent tres. For the collection of samples clean plastic containers with a capacity of 500 mi or 11 are suitable. They should be rinsed with the water to be tested several times by shaking vigourously and after airight filing should be closed well, 1.2.2 Pre-testing Correct results will only be shown within the measuring ranges given in chapter 1.1.4. If tho rosultis up to 10% higher than the upper measuring range limit, the resut will bbe marked with", Even higher concentrations ws i the display Heese". In order to prevent incorrect, doterminations the numerical values are not displayed. Submerge the test strip wit ‘he reaction zone nthe water Sumpter secon. to dilute metal compounds which are otherwise difficult 0 lute, but, on the other hand, make analytical detection of the metal more difficult. Tne eubstance to be tested can also elude analytical proof due to the presence of solid sua- stanues in ie fon of fakes, eg. metalic hydroxide or colloid, which the human eye perceives as a clear solution, In addition it must be guaranteed thal the concentration of the substance to be determined is within the measuring range of the method eelected and that the optical pH range far colour formation can be achieved under these conditions, Incividual or random samples can generally be taken by hand by direct filing the plastic container. In any cases a real picture of the average composition ofthe water is only ‘produced when several inawviaual hand collected samples, are mixed together, or ae collected by automatic sampie collecting devices. Here it must be taken into account that the resulting mixed sample can change during the course of the sample taking, For this reason the sample should be pre-treated and measured as soon as possible. \When working with sample solutions of unknown concen tration, the user should establish ifthe sample concentration is within the measuring range by using suitable pre-test, Tires incre ative reliably atid rekes eterrinali Of the dilution ratio necessary for high sample concentrations easier. Merckoquant test str for the semiquantitative determination of water borne substances are very suitable as pro-tests ‘Compare the colour ofthe reaction zone with the colour scale. Read the result. 12 4.2.3 Dilution Generally, if the concentration of tre substance contained inthe water is t00 high, a solution which is to0 intensively coloured results, During the measuring process the SQ 118 photometer signals thal the measuring range has been exceeded wi+++44% The sampie must be diluted porore the analysis and addition of the reagents, Required for this are: piston pipotio, ‘© measuring flasks (50 ml, 800 mi, = istilod wate For reasons of measuring accuracy the dilution should be Caleuiated in such a way that the dilvted solution is, as far as possible, in the midcle of the measuring range for the ‘olactad analysis method. If tha mathads allow diferent ‘measuring ranges the largest possible measuring range ‘should be chosen in order to keep the dilution as low as possible. Example: A concentrallon of ea. 40. mit Cu is expected from rinse water containing copper tram semiconductor production. How must dilution take place? Largest measuring range: Method 108 Copper measuring range: 0.10 ~8.00mgii Cu Midale ot measuring range: ca..4 magi! Dilution factor 40:4=10 Through the selection of the sample volume ang the moasuring ‘lack various dilution factors can be realised, 20 ilustrated by means of some exemplee in tho ‘ellowing table 4.2.4 Increasing the concentration If the concentration of the substance in the water is below the measuring range, adcition of the feagonts produces a very weak colouration which can often barely be cistinguished from the blank with the naked eye. A photomeier can also only measure very sight concentrations with a relatively large error. With the help of special enrichment techniques, e.g. the use of lon exchangers, extractions, etc. concentrations can be achieved which Ife wittin the measuring range. A simple possibilty is offered by increasing the concentration by ‘evaporation of the sample solution. This method promises success wren: ‘© the substance ie not changed by heating, ‘¢ no parts of the substance evaporate, ‘+ 0 condensation containing the substance takes place during the evaporation. a ‘with distited | tion ution somple | waterto factor umber 0 som 5 4 5 som w » 2 50m 2 2 10 0% 50 ® 6 som 100 ® ‘Alter filing with cistiled water the measurement ask is ‘closed with a stopper and the contents mixed. The analysis, is carried out with the diluted solution. In the SQ 118 pphotomeier the input of a dilution number is possible. ‘The dition number must be in whole numoers between + and 99, The dilution ig entered in the forrn "1 + dilution number. The cilution number represents the volume share. af distilled water, Example: + + 4 means 1 part sample + 4 parts water For samples with fully unknown concentrations a pre-test, 8.9. with test strips, can be helplul for establisring the optirral dilution. This applies, among othor things, to weakly acidified water with a low total hardness and slight sal pollution In such samples, for exemple, on and manganese can bbe determined using this technique. Example: The manganese content of ground water with litle calcium should be determined, Approx. 0.05 mail Mn is, expected, Most sensitive measuring range: method 45 Measuring range: 0,01 ~ 2.50 mg/l Mn Sample volume: 400 ml Volume alter evaporation’ 10 mi Concentration ineroasa factor, 100: 10 = 10 Analysis of the increased concentration solution showed (0.40 mgit Ma, Conversion: 0.4 mgf : 10 = 0.04 mgf ‘The ground water contains 0.04 mgf! Mn, MERCK 13 1.2.5 Differentiation of forms of appearance The substances contained in the walter of the test appear in different forms: as ‘complexes or solids, ten comple ‘oli ee forms can be cif means of a ‘sample pre-treatment. This will be illustra waste water by the example of waste water containing copper. tained by a digestion of + The total content water sampie (result A) “ual ‘+ Solids contained in the water sample can be seperated filtration by fitraion. A subsequent digestion registers the compiexes and ions (result 5) } + Alter fitration ofthe waste water only the ion share presen under the reaction conditions is registered digestion digestion filtration (rosuit ©), cuioH comple: C-EDTA complex Cu-EDTA one ‘oneute ion cut rout A oo eau shee oid substances: 1.2.6 Filtration Water sample components contain the substance to be determined On the athe arbonates, sulphides truer . to distinguish be disgoived and undissolved ‘gher molecules, et substances (eotd subst jakes can be separated with a simple fier paper (blue band) sasurement more dificu Fol ward (DIN) a customary surate results. The coloured membrane fiter with a pore with of 0.45 jim is used re usually not completely clear. They must bo clear, Turbidities must be removed by filtering 1 filtering af the water sample is used Turbicity makes photometi sand, @8.a rule, leada to in solution prepared for measurement in the SQ 118 photometer for fin KAT ‘ptomntauon ernie fusion Sere ine nme iy one Hold he syringe upg and ‘ner ue contents oF he yringo Drow out the gu toe trntace ofthe memiraniter How peas thud ypards_‘nothwilended ian ans fitered vith a syringe. ‘mombrane iter is achieved MERCK 14 1.2.7 Digestion Certain metal ions, @.g. Cu?* and Ni2+, have a particular preference for forming stable complexes, The Cu-EDTA complex, for example, shows completely new characteris tics in comparison to free Cu2* ions cue to the fact that the ‘conttal ion Is surrounded by a “shel of chemical groups land is not accessible to the colouration reaction. Proof of ‘copper, therefore, can only be achieved when the “shell” has boon destroyed. This process is called digestion. It transfers the complex into the relevant ion (Cu2+) The necessity for digestion can be checked according to the following diagram, digestion implementation measuring process result A All digestion lakes place by means of boiling with acids and oxidation reagents, in part additional catalysts are used. The digestion processes aro dopondent on the substance. If the cigestion mixture 's reduced to “almost cry’, care Trust be taken tral the residue reer slighlyrsutst Inthis way it can be more easily diluted with distiled wator. By overheating to the point of absolute dryness the residue loses its solubility as a result of chemical changes. Cu® + oxidation products implementation measuring process, result 8 eS digestion necessary ‘The sample can ke analysed without fitering, once with and fonce without digestion. Ifthe results A and B are equal within the framework of measurement accuracy the digestion can ‘be abandoned. In the caso of clear differences in the results, 1.2.8 pH correction Chemical colour reactions only function optimally n a very distinct pH range. The use of Spectroquan: reagents leads 20 a buffering of tho eample golution and, in gonoral, to tho optimal pH range. Very acid (pH <2) or highly alkaline (> 12) solutions, as well as those with higi salt content can disturt the optimal pH value ad|ustment. Then the Dutfer capacity of the reagents is nat sufficient. In the analysis metnods listed in Section 2 0 this manual recommended ranges are given where a check of the pH value is useful. The pH value can be checked with pH Indicator strips, Annecessary correction is carried out drop by drop with ailuted sulphuric acic 0.6 mol (owers the pH) or with diluted sodiurn hydroxide solution 1 mol (raises the pH). After each no Aand B yes the same? no digestion necessary the sarnple must be digested. For waste water having 2 com- Position which remains the same this double determination testis, as a rule, only necessary once. It should, however, be checked periodically top the solution should be thoroughly mixed anc the pH value re-tested using the same indicator strip (submersion timo a minimum of & eoeonde). Tho addltien chould be: repeated untl the optimal pH value is reached The original solution is diluted during this correction process, Incase of the addliion of a large volume of sulohuric acid or sodium hydroxide a volume correction Is necessary for exact measurements. Where the starting solution was 10 ml and up 105 drops were added a correction is not necessary as the ear lies under 2%, Adcitions exceeding this amount must corrected appropriately for tho volume. MERCK 18 1.3 Hints for measuring practice Information specific to the method can be found in the: leaflet enclosed in the respective Speotroquant package. Included are: Colour reactions The fundamental chemical methods underlying the respective Spectroquant reagents are explained In short, This knowledge can be important for the evaluation of the resus and for comparison fo other analysis procedures. Usage areas Here the form of the substance in the water which is being Getermined and sample material which can be used are described. Advice concerning the sea water sutabilty (of the fests is also given here. Influence of foreign matter Accompanying substanoes in the sample solution can lead to similar cotour reactions or innipit the reaction. Turbiaty ‘can also lead to deviations of the result from tne real Concentration. In such cases the colour forming reagents react, not only with the supstance to be determined, but also with other accompanying substances and, as a result, the calour formation fails to take place. High salt concen- trations can also iniluence the colour formation by interaction, Quantification ofthis effect, which can lead to a distortion of the result, is given in a table of different foreign rnatter. The tolerances for each ion are cited individually, They may not be cumulatively evaluated. 1.3.1 Thermoreactor TR 300/TR 200 Sometimes samples have to be heated using a thermoreactor The information obtained is not only important for obtaining tho COD values required for controling waste wator, itis also necessary for determining total phosphorus, total ntrogen, total cyanide, to:al metal determinations of chromium, iron, nigel, copper, zinc and silver. Further application fields of the thermoreacior are the analysis of sowage piant sludge and extracie of piante and eoil samples in aqueous solution. The application procedures, which you can request ftom us free of charge, contain a Getalled desoription of each sample preparation with the thermoreactor. The practical Quick-Fill cell rack puts 12 reaction cels (TR 300) respectivaly 8 reaction cells (TR 200) simultaneously at your disposal. After fling, the rack is placed into the: thermoreactor. A special isolation technicue provides ‘optimum working afoty. The epecial cover means thet all paris which are open remain in a temperature range where there is no danger. The safely id offers adaitional protection incase there should be a leak MERCK 16 Reagents and aids Horo the contents of the Spectroquant packagos, as well a olher reagents and attachements, which may be required ‘or the preparation of the sample, are listed Preparation Advice for sample proparation is given concerning whieh tests ate suitable for pre-ovientation. Digestion takes place by means of boiling with acids and should be carried ul with proteciive glasses under a well ventilated furehood. Absorption spectrum The absorption of the colour complex which occurs is dependent on the wave length of the light used. A graph of absorbance against the wave length is called, in short, spectrum Stability of the colour complex ‘The stability of the colour complex is dependent on the temperature, as weil as the duration of the colour reaction In addition, advice for process monitoring and waste management of the reagents is also given Inthe sample analysis, you can choose between temperatures: TR 300 s 100°C, 148°C TR ono we sna TANG, 14ne, The in this manual indicated data of 120° C (100° €) means, that the cell should preferably be heated up to 120°C. ‘Asan alternative 100°C can be used too, ‘Tho working temperature ie reaches ator 10 to 16 minutes, Attention: The cell should be inserted into the up to the indicated temperature pre-heated thermoreactor. The timer, with a remaining time display and automatic suwitch-off mechan'sm, permits a tree choice of reaction time of up to 120 minutes. Satety is further provided oy Control lamps for power and temperature and an integrated protection against overheating. After cooling in the Quick-Fill cel rack, the sampies are ready for measurement 1.3.2 Piston pipettes Pision pipettes allow exact cilution and measuring of sample volumes, Three models are available. 2 variable olpettes (05-25 mi and 15m), each having § fixed volumes, as well as a piston pipette mano 3 ml, which has been specially dasigned for the call test method for the determination of the chemical axygen demand. The tips and sticks of ‘each pipette are made of high quality polypropylene and can be interchanged. Tips and sticks are packed in a handy 10 pack Principle of crect expulsion 1.3.3 Shelf life of the reagents “The Spectinqniant tast sets ean he kept tne at inast 2 years, f stored coo! and dry. Some tests are marked with Iminirrum shelf ife. Reaching this expiry date does not conclusively mean a lass of usabilty. A function test with a standard solution is recommended. Piston pipettes function according to the principle of dire liquid expulsion. The sticks pushes the liquid directly, without an air cushion, causing the inner surface of the syringe to be wiped thoroughly. This eliminates the poss billy of wetting with remnants, Prerequisite for exact dasing of the amounts of liquid is the cortect adjustment of the o'ston pipette. The individual steps can be found in the pipette operating instructions and particular attention should be paid to these. In arcier to Prevent errors resulting from spreading the tip of the piston pipette is rinsed several times with the licuid which Isto be tostod and the rinse water discarded. This is particularly important for dilution steps. ‘The tip is to be tiled without eir buDDIOS by slowly drawing Up the plunger. After the pipette stens are completed the tip should be rinsed several times with distilled water and after frequent use it should be roplaced, Alter ramaval af a reagent the hottin shill he closet immediately with the screw cap. Evory unnecessary contact, with moisture shortens the shelf life of the reagents. MERCK 7 1.3.4 Dosing the reagents ‘Small amounts of liquid are dosed by counting the craps. ‘rom a leakpcoot bottle. Larger amounts of quid in the mn range are dosed with a Piston pipette Honing Dette as far as possible into the pipette 189° so that the piston Se botl oro position. Pisce the piston Pipette emiy on the eakproot tachment ofthe bot, Powders are measured with spoons o a particular size Coloured spoons, integrated in the screw cap, are used small amounts, There are four aifferont sizes, 03m! (red) O.1mi (blue) 0.03mi (green) 0.01 mi (grey) 1.3.5 Blanks For reasons of accuracy against a blank, Tho blank compensates for the intrinsic hresuits from the addition of reagents of the corresponding amount of cistiled water easuring generally taxes f MERCK 18 (eal When using a dropping bottle It's absolutely important thatthe bottle be el vera ac pe ye. ro pr sarc. Oterwise te ‘wil be incoroct, mer raw the stick sowty down to the requred volume orentaton: Upper edge ofthe sek inal. Contents ofthe pipette should bo prossed back into the bot and {he ng process repeated. After filing without er bubbles the ‘shout be tumed 180" to the ‘rginal position. The filed pipette Should be removed trom the attachment on the bottle and the tid carci putin he eaton Handling: * Transport the powder to the botto tapping lightly on the otto. of the bottle by + Take a well he powder smoothiy on the i pe off the excess go of the bot, ed spoonful and * Close the bottle immediately with the sorew cap attor remaving the powdar id to the sai forthe most part 'e solution and already contained in the can oe used repeated 1.3.6 Influence of temperature In general increases in temperature accelerate the speed ofthe reaction, however they often reduce the stabilty of the calour complex. As a result the temperature has an influence on the intensity of colour and, therefore on the result of he analysis, For exact measuring the samples 1.3.7 Time dependency Most of the colour reactions requite a certain reaction time to reach the maximum intensity of colour. The reaction times given in the description of the analysis methods in section 2 of the manual rler to te time period from the addition ofthe last reagent until 1.3.8 Cel and glass devices ‘An indispensable prerequisite for a high degree of measuring accuracy is clean work. All devices used must be clean and dry. Immediately after the analysis the measuring flasks, pioettes, reagent vesse's and cells used rust be thoroughly washed out with water anc finally with distiled water. land reagents should ire at room temperature (20-30°C). As aruie below 15°C will produce inadequate results. ‘Advice regarding the allowed temperature ranges is included in the enclosed package insert of the Spectroquant test > Phosphowus 14846 . 20 20 20 Silicon 14794 . 2 5 2 Siter 44831 . maitrange 1 5 Suphate 44791 . mgitiange | mal-range - Sulphate 14848 . 10 2 - Sulphate 14564 . 10 20 Sulphide sara . 05 1 1 Suiohite 14304 . 2 20 20 Zine 14892 | 5 18 Zine 14866 e | 10 MERCK 20 1.3.11 Measuring high concentrations Correct results will be shown Ifthe concentration of the sample is within the indicated measuring range of 2 metro ‘Asarrul results above the measuring range limit wil be marked with a "+" or the display shows "seee4+" ‘There are also cases in which the absorption measured decreases again with increasing concentration. These cases re by far beyond the validity 0! the Lambert Beer Law, When measuring very high concentrations (drastically exceeding the upper limit of the measuring range) the tests indicated opposite can show compiotoly different colour reactions with the consequence that results are shown within the measuring range. These results are wrong, Up to the concentrations indicated the display is correct. ‘Apove these concontrations the display is wrong because readings are shown 2s being within the measuring range. In this case a plausibilly testis necessary through e.g, dilution or pretesting, 1.3.12 Safety hints Please pay attontion to tho risk warnings and safely advice onthe labels and rezction cells! As far as possible the fenoiosed ieatlet contains additional safety advice ax appropriate. Gat No] Method Corect | Comment resut untl | colour change cone, 1782 | Ammonium 28 maf | wurquoise instead of green 14558 | CT Arreonium | 250mgf | turquoise instead of grosn tasag | CT Amonium | toomgt | turquoise instead of green 14559 | OT Ammonium | S000 maf | turquoise instead of green 14828 | Chierine somgh | yellow instead of rod 14857 | CT Fveride Amal | prown-yetiow ins, of volt 14853 | CT Copper 25 mal | sahteleruzquoise net of bi 14767 | Copper 25 maf | ightolve/turquoise ins.of biue vassi | crPhencle | too mah | colour weakening saeat | siver Sinai | pa change (precipitation) MERCK at 1.4 Quality control vaiity control in analytical chemistry Is concerned with ‘he question: How "reliable is the result? In general, ‘measuring the same sample repeatedly will not produce exactly the same result. As a result of coincidental influences faven with very accurate work the reeult wil fluctuate around amean, Example: AA determination cartied out 4 times on a standard chromium solution with 0.50 mg chromium produced the following results ©, =0.48 ©,=051 6-040 Because the results are ciforent it's not possible to say hich is the correct one. But it's probaoie that it les somewhere in between the individual results. Where is determined by the erthiesc mes Arithmetic mean F = : the sum (2) of the individual results (C)) divided by the number of the results (r), _ 0.48 + 0.47 +051 +0.49 4 = 0.4875 ~ 0.49 mg/l Gr Accuracy (A) = : the moasure ofthe deviation of the mean (©) tom ine contol conceniration (C,) with reference to the Control concentration For a statistical description ofthe results a second quantity is neosssary in addition to the accuracy. This becomes clear it \We Nad got the following results from the determinations, ©,=0.52 The same mean of 0.4875 « 0.49 mg/l Cr is obtained, but the individval rosuts oitfer more extensively from one another. Between the largest and the smallest result there is a Cifference of 0.08. In the preceeding example the altference wwa9 only 0,04 mail Cr ‘The extent to which the results ciffr from the arithmetic mean is defined by the standard deviation. For the original values the following resus: Standard deviation (8) = the measure of the mean variation of the incividal results [ae axara® 074 0a079? + 51-079? 6A —0407a? =0,0171 By procieion io undoretcod the measure of agreement ‘between the resuits obtained irom the repetition of an esiabished analysis procedure, Itis described by the variation coefficient (VC) or the relative standard doviation, Vartation coeftictent (VG) = «the rallo between the standard deviation and the arithmetic mean, 90171 0.4875 100% =3,5% ‘Accuracy and precision are important statstival naramatars ‘or the evaluation of an analytical measuring procedure. MERCK 22 1.4 Quality control To usta the target is rentration. The indivi ts: possible large error (00 hits) precision bad accuracy bad coincidental errors: precision bad uracy good ) systematic error (oo hits} precision good accuracy bad result very good precision good accuracy good is a target serves as an example. The centre of ual Fits indicate the values. The following illustrations show four Precision bad: The hits ate widely scattered ‘Accuracy bad: ne hits are a long way from the centre, Precision bat No gross errors, but the hits are widely scattered, Accuracy good: tn the middie section the hits are regularly dispersed around the centre Precision good: All fits lie close to one another. Accuracy bad: ‘Although all hits lle close to one another, ‘the goal (contol value) has been miss Precision good: Allhits are clase to one another Accuracy good: Allhits lie clase to the cen! ear the control val hat i, MERCK 23 1.4 Quality control From the parameter accuracy the folowing can be recognised: Gross errors Results which cleerly deviate trom the expected concen tration and strongly from one another and simply cannot be correct. The accuracy is bad. Causes aro, for example, incorrect pre-treatment of the sample, incorectly measured reagents, etc. ‘System errors Numerous determinations produce very close results which, howovor, deviate from the control concentration as a result of a repeated efor. This is @ system error, the cause of which lies in e.g, incorrect keeping of the reaction time or a pipette which has not been correctly adjusted, From the parameter preeision tho following can be recognised: Coincidental errors These erors cannot he completely avaidied. Thay can, however, be kept fo a minimum by good working techniques. 1.4.1 Measurements at the lower limit of the measuring range The measuring ranges of the methods are determined slatistcally rom measuring data. Within the measuring range reaults with an accuracy of better than 89% can be main- tained. Each photometer shows a more or loss large result deviation from the true control concentration. These deviations are specified inthe technical data In the first ‘approximation one can assume that with small absorbances of A. 5 6 =A SA = ons Plsathe ankce inthe eel pass ih Decoufonsto septic cri Spare ‘ press te (CT ey come pt te sane pei Ener the mod number Sweatt ange: nH-8 Presb OL) bs 6 cops nd. evoke res the Cia. he lanka sae. ‘The est pps nthe ope MERCK 46 Formaldehyde 14678 HCHO Cell (0.02 - 1.80 mg/l HOHO 0 4.00 - 9:00 mg/i HCHO 10 Pipete8 mcFHCHD-1 in aac of A grtn ncronpont of Shake un tb agert's lest es, eosethe data 1 of aid wate into ace the bank cal ite cel corps MERCK 47 Hazen colour ‘Memod number _ Measuring range oo! is? 2— 200 HZ 50 138 10-1000 HZ 10 Enter cptinet Prete MERCK 14797 NaH4 Method number Celt a 0.02- 1.00meI NA 50 38 920- BoomanN: io 39 08 = 312 mmrolf 50 20 8 158) mmoln 10 pete 10m mnt rokgesecwse Ais Depathy-Atea Aros 2A Presse ier ay. Recon i at 2 nS se MERCK [Speomoquant a lodine colour number Method number __ Measuring range cell 135 136 at ° ai sat MERCK 81 14761 Teen) Celene RNa Fe Method number Measuring range cel 2 — 4 rn 3 2 3 50 36 $6 =480 mmovm re 20, Om dstted ter AS Aocach Preset bank ae Hey S TA Bl! 0 the tina. Reaclon When einer ep of mints beg ttecoldons oan pres te ES) ty The rest npr the day Pace te lank eine ol MERCK ; Manganese 14770 - Mn ‘Method number % 2.50 mail Mn 47 48 2 mmoviee Mn 2 4 Praotte alco cl corparent MERCK 2.00 mgt N 05.00 mail N. 4.0. ramol/m® Ni 5.0. mmovin® Ni Pace te loin all Nickel in electroplating baths Ni Talatoccalaeeelels Metnod number Measuring range cet 167 10~ 120 gf Ni Pass th (I ey. 1 lnk ae is cep MERCK Nitrate 14773 NOs Method number __ Meaeuring range Col!__—-Mathad number _ Measuring range cal 5 10 ~25.0 mg/l NOS 30 a 16-403 _ mmovm® NO; 60 5 38 =800_ mo Nos 0 33 8.00- "S4smarme NO, 70 3 825- s85mpINO“N 80 Ed $397 20.8" mgr NON ° Aircore Sandy aw Sate ager enter ee Solitons to seperi amor the arkcal fom'te aeons MERCK Nitrite ‘Method number Measuring range cot Method number Measuring range cet 2 10.020 - 0.600 ma/l NOs &% (0.4 ~ 18.0 mmov/n® NO 50 0.05 ~ 3.00. mgf NOs or 110 65.0 mmol/n NO: 10 Pate Omani Ppete Do ns 2b mi ros te lank val mglesolto—ifoastoand ee (oink Belt one and zak, reste oo soit str an appears in MERCK Phosphorus (PMB) Coda tare alee) Method number __ Meaouring range colt Method number Measuring range Ca nm 50 x 005- 230mg BO, 50 0 02 ~ 115 moll AO, io 06 - 923 mmolm#PO, 50 3 mmovm! PO, 10 sete wi ns ta separate cas compaiment MERCK 60. 14842 Method number z jeasuring range con 0 0 MERCK et 14794 Si ‘Method number Measuring range cet Method number __ Meseuring range Catt a 0.010- 0.800 mgi Si 20 as 03- 285mmoymeSIO, 50 2 0.10 - 5.00 mgiSi 20 8 22178 mmoym SiO; 20 3 002 = 1:70 mol SiO, 50 98 02° 10:7 mgiSio; 20 Poste 10 lof te sanpleito Ppt 10 lf ase waar asthe Hank a iettobe amie solten) oa sacondest nee (Oark ade st uti Reactn relator. eas ln =p neds ch Preset tary. Reacton me When he Pas he nk ca nthe al kl rom bo ross tno CI a. he res appears inthe ply MERCK 62 Peete 14831 t Ag ne | Ere 14791 x sox Metod number Measuring range me | inet) 14779 s MERCK 65 Measuring range 70-400 NTU ei OC! a nie 3) H yl os ei oe ym, Oa, S =a wom Setar meni uit Oe MERCK . __Spectroquant- . __Cell tests Ammonium Meee Cell test Method number __ Measuring range colt 28 02 100 mol NHt Round 127 0207-80 mg NHN Round cl oft salto a Pres thank ae econ be, or Cag wt ha serewcap and ma Pres te ere. eaeton tna When the ohms bis MERCK 70 Ammonium Cell test Method number __ Measuring range Cel rn 1.0 -28.0 moiNHi Round 2 08 217 malNHN Round 3 "755 molin® NHF Round Pres ei Rae ne Fi mo (se th he aru cap and a robimoa fad nae Kuso cre op Presetne CS iy. Da SS) rene an ieee, plae he ca hae sere 2p the taco hm eal emote nec cattrmive — passine (I sy To aut appasin te dspy MERCK 7 Ammonium Zo is (eae Method number ng range colt 128 5 = 100 mg/l NR Round 123 4.0— 78.0™mg/ NHN Found react cand sang Vor ‘Press the timer kay. Reaction time Pr fore MERCK 72 Cadmium Cell test Method number __ Measuring range Cel 18 (0.025 = 1.000 mgit Ca Round 2 ti mA 4 hse pit ote sample. Speci une: 5-2 “[: Sheol eraagent MERCK 73 6 Chloride 14730 # ‘Method number Measuring range Coit 160 5 ~ 125 magi Cr Round Prats bk ay Prost re ospay MERCK 74 Chromium hexavalent ec as Method number Measuring range Celt 108 10.05 2.00 mg/l Gr Round 46 ops of eto ‘cazon cl Gaeta any fort mine Stale te ol and xt aie Greate nirme pe, Hn ks vt Speed ng opty opie auth d me Masmlimesinge Cott Fess every Presse tmeriey.Rsciontine When hetinerleps, 936 este [EI dy. frenitoy se onan oe a crane poste CD MERCK 75 Spactroquant : o" Chromium om [ total-Chromium, tri- and hexavalent Cell test Method number Measuring range cet 108 10.05 - 2.00 mg/l Gr Round eed sample As ro of Ck logy fd mi coD Chemical oxygen demand 4-40 Method number __ Measuring rango Colt 2 “40= 40,0 mg COD Round MERCK cop zoo Chemical oxygen demand 10-150 Method number Measuring range Got 28 10 150 magi COD Round ow rit te sare Slulon roa ean el ane ign sea on he Mic CAUTION enn cal on ot ‘Wat url Raton me "ease an eden, saree Faeve te nko rom the faeompanmart snd aa te ‘ao MERCK 78 @ * cop wo s t Chemical oxygen demand 50-500 iz Method number __ Measuring range Cel 8 50-500 mg/! COD Round Hath action clin her Imactart 8% for? Nos empeatre (oat ast Press tho Ct. The es apna inthe 9. Pace ark cal ite seen ess tn BET by capinneealcomasnen atin res la MERCK 79 coD er Chemical oxygen demand 100-1500 (eco ‘Method number _ Measuring range cet Ey 100 ~ 1500 mgil GOD Round rst (CT) ay. Etre mae nb Presets By. oss tho (dy. MERCK 80 cop om cH Chemical oxygen demand 300-3500 Method number Measuring range Celt 749 ‘300 - 3500 mg/l COD Round MERCK 81 o Method number 108 (a) Pres the (CH ty Estar med numb Pras te sey Measuring range cell 0.10 8.00 mg/l Gu Round Copper Em rT 5 erops of CuK, case ay 0 #requed, 8 ae amo'a salon arp by capo aust aot roe tho GD . The st appears in tesa. Pros the ray. Racton ie cast bois MERCK COD Mei) Chemical oxygen demand 500—10000 eRe Method number Measuring range cot Te ‘500 = 10000 mg/l GOD Round Hestneeason cain henna: Remove tie fromthe Saket al ate 10 ross the (CZ) ty. Seon iC trdhom. fetiebicrcpas nara pi eA Ce cher Samat ross tne (I a. FeovetheDankee om he pres ine GES) ty Siempre ant "este GED Sarpocl ath vara ing TO OE inte dy. fang he ober MERCK 82 Cyanide Mehl freely Cell test Memod number Measuring range colt 110 (0.025 - 0.500 mg/l GN" Round eospy. MERCK 84 [Speszoquant Cyanide readily released Cell test Method number _ Measuring range cou v0 10.025 - 0.800 mg/l GN Round ds MERCK 8 i“. @ Fluoride Leads padll Method number __ Meseuring range: cot 116 010-150 gl Round the (EZ) ke bees, rua, a i ti ea meen ot Senta age poet on ry op Fk. Close win sre ap ti rte sen pe eee foes ny a “ fr beara atone Whe hee es Puss the [I ay Fem te lak cet rom ne Seater Snes 3) calconsuartnd ste compartment wine veea "Ditka is dspay. Sang er nn te vrelnt ine toca te observe Inena te abs Pras to (°C) ky. Th stapes in te py. MERCK 86 Formaldehyde er ‘Method number Measuring range Cell 720 0.41 - 10.0 mg" HCHO Round ‘peas Presse er ay. eacton tine When of Sins topes an Fano om dereet tome paste ty. evartealane Tce appears inte display. MERCK a7 peat ; Hydrogenperoxide Lat , Method number Measuring rane eat 15 ~ 20-20.0mgiH:0, ~~ Round prs tne heres appears he a. MERCK 88 petroant | Iron Method number _Measuring range _—_—Cell ‘07 0.10-400mg/ Fe Round = St hao eit pote sane Soe ange: 2-7 Pros te tiner ky Ratan ins Un Sok unt he anes Press te lanka ain Reset eo an apes e Presto MERCK 89 tae Lead 14833 ri Method number Meusuring range colt a 0.10 5.00 mg/l Pb Round Total hardness 0-17" TFT o esl ss] pressive (CX) toy Cock hares sample, Check ote samp. rage, ad ve sadum A ops of PK to . 7 Specs ange: S38 Fyodor ose a6 reaton el Case wit he sew Entec the meted ube Stop crop oases capa mic Pres te () a =a =) 4 SA FiuSmiottresamaleintoa Press the Yank valu Pett iankcel (ite sro pass te GS) sey cu WatursRaacon neo cp) toca camparmet AS bse wi the serewcap ands, "Measure lark apprarsin wither ine acrg be TAnkyaeS USehve. Sampo iss sasener ‘aang iw oben prste BED es Theresa Aappowsin the dsp, ‘Total hardness > 17" gf Pb = Result A~ Result B Oper reaction cet of vale A Shake athe agents sanplecetin teal peste GE) ky Caleton of ead comer. fia or mieesoontlet assed tempstrert nt he vec ing estte CC) bey Prox tno eon fachg ie asa, esol 9 npr in te dpi MERCK 90 xe | Nickel eo Fai af locos Metmod number __ Measuring range cel 108 (0.10 6.00 mg N Round kclostte Pest timer by-Redton tine When the tine 1 2rinaes bones, i MERCK 92 eoraar Nitrate ‘Method number __ Measuring range cet 59 80.9 mg/l NO; Rouna 60 180mg NOyN Round 6 32° 1290" mmolims NO; Round Pres th tne ky React tine hi) meus bos MERCK a” Nitrate Ud He 2.6-Dimethylphenole Method number Meseuring range Colt 180 2 = 100 mg/l NOs Round 331 0.5— 22.6 mg! NO;-N Found FULD mvt sample ie the Add 1.0 of MK. Pst Pras teint hy. Rectan tere ce ee waotesanighrsceves Tetlystewenberapanic Waitin Resonting: =» tome Presse (ey tedopay Caicoreanmenaa norte Pest" GED we ee tee Tora appt nthe py tage obser MERCK Nitrate (eR Method number Measuring range 117 05. — 15.0 mgllN Round 118 O11 340 mg/IINO-N Round 119 8. =242 mmosmsNO; Round oeSinnie enh Wren tgs rt ne Fevovetn tink forthe ons GES) MERCK 95 Nitrite Meee eae Metiod number Measuring range Colt & 0.05, gil NOs Rouna 68 0.020- .6tomgANO;N Round 70 = 43.5 mmolmNO; Round (2) Pras th tna by Recto tne eames tgs Press ne (CI) ty Ener te ato aba Pree» I dey lace the pce he (I =D)E tan depts Theres appar inte dspay MERCK 96 "MERCK 97 re ” Phenole sd Method number Meesuring range cont 1m (0:10 - 2.50 mg/l Phe Round echt fe sai. sonia tea 41 gy merc Speed ange: 5-3 ional Chsreth scien OPH bapa it ite eng r Sha nthe regents saved ren ctssovee MERCK ae! Phosphorus (PMB) oe ortho-Phosphate Method number Measuring range Coll 73 QG5- | 50mar FOP Round 80 02° 183 moi PO Round Bt 84 = 18 monpe, Round cA 2 =160° mmol! po? =r 2g6 ame sin. rb a MERCK 99 Par Phosphorus (PMB) Eis Total phosphate (eR ‘Method number Colt ia 80 89 Round Found ound MERCK 100 ae” Phosphorus (PMB) | ortho-Phosphate (or crcid Method number __ Measuring range cet 40-250 ma/l P,P Round 18 31-788 mai POL Found MERCK 101 4 Phosphorus (PMB) 14729 | Total phosphate Method number Meaeuring range Cott 2 1.0-250mglP Round 143 3.1768 mgl POS Found Cathe ct and stake to dao te powder Se ero theta MERCK 02 pat 7a Phosphorus (VM) om cH ortho-Phosphate Method number Measuring range Con a7 0.5- 25.0 mg! POcP Found 88 15 — 77.0 mg! POF Flourd 89 1-1~ 57.0 mgf P.O, Found 80 16-807) ey Por Round | Sat © the lank vale ey the lonkcol ite sera prestie FES) ky. Matt Raton be yr th la aa rsa ine fag be The nk value ised Feros the nko rom the Coteogareent sd na te snp el with ever he MERCK 4ng Potassium Md Cell test ‘Method number Measuring range cau a1 50-500 mglK Round Cage econ et ane sisson by sang vars Shut bt shee MERCK 104 : Residual hardness Mec | Method number Measuring range Cell 158 0.075 0.750% Round 187 050 5.00 mo/iCa Round YY Press the lank vale ey rs the te ky-Reseton tne Reason tn rors mutes beh lan pps tedepby. treetn (CE) anh set tera iy nb nan te be ao rani Sepa preset (ay MERCK 405 as” Sulphate Me ‘Method number Measuring range oct or 20 240 moll Round 98 021-" 2.50 molim® S Round Hust be tere. MERCK 106 Bpectroquant Sulphate St Method number __ Measuring range Catt 133 100-1000 mg/l SOF Round rau the (I ay. a su appa nea. MERCK 407 Sulphite km Method number Measuring range Catt 134 1.0 - 25.0 mg/l SOF Round Presto timer, Reacon tine “0 a She ear am or2menes be MERCK 408 a Surfactants Mes Method number __ Measuring range con 4 (0.05 ~ 2,00 mg/l MBAS Round Vraqited. at testohm Smal hesampemtox Add Cops ot 1K Dont mc Tyrone stor orien atten el Do not Sei drop by ft the a2 cops 2K rosy Peto Whe i ies to eat for 90 secon en MERCK 109 Tin zm Mothad number _ Measuring range Call we 0.10250 mg/l Sh Round hehe pit o rena, Spel ge pes (CE facing te bse Pest 7 appa inthe dsp MBRCK 110 Total nitrogen er de feo R oe Method number _ Measuring range cot 140 05-180 mgiN Round ‘Sample preparation pv’ StS aed tet MERCK 2 Zinc | 14566 | lec Method number __ Measuring range cen 105 020-500 mall Zn Round rT EF CK Jom f°) oe res the (CZ) ack te po te samp sags cops o2n-tKivios Red O5 of tesa ic) Sorc range: 95-8 hye Stor osu ac rae et and mi oe hcl igh an op ap fo ast eo Enerte nad runber, Pras the OE sy fc = = Bl Add crops of 21.26 Pras teak ale hanno siecle, 58 the Presto» (TS) ey. Giue tees toy anemia "Becton tine" or alan cl (we scr eat) ne sere bn sop Teormarnet the yrs Tetirk alos aspaye tw dep maf he oan yee lnc om he calcangatren as Pee ea apr ty fac MERCK 113, EM uka ees Rees 3.1 Description of the instrument The SQ 118 is a universal standard photometer which can be used for routine analysis as well as for the well-directed solution ot more compiex tasks. This functional versatity has been achieved by the consistent use of the latest micro: rocessing technology. Optimal software in combination with microprocessors and other electronic components ‘conto! the setting of the instrument and the data processing 0 that a maximum of user-riendiiness is guar a the movements necessary ‘or carrying out a determination ave been reduced to a minimum. The SQ 118 is spec ly adapted to the analysis methods formulated for use with the well-provon Spectroquant tests, The data ofall Spectraquant tesis, such as factors, neasuring ranges, units, etc, ae fheorogremmed. Inadaition user-generated methods can be entered to solve ‘special formulations 3.1.1 Installation meter should be installed on an even table fensive light 0 jaw in dust and smoke. he esvironmental air should b The $Q 118 isa single beam photometer. It functions with a tungsten halogen lamp and a filter rotor with a wavelens range of 340 {0 820 n™m. The ther Is autornalally p inthe beam path ved The easily acc for 10, 20 and 50 with an oxter ile cell compartment has been conc im rectangular cells and for round c of 16mm ‘Measuring data Is saved and can be printed out with a customary printer. Every result is documented with the fe, ime, sample number, and the dilution entered and 5 data specific to the method, The SO 118 has a robust metal casing end can be run from 1 ysis. luded are a connection cable for replacement lamp and battery operation, a dust cover, he device works in an environmental temperature of between 10° and 35°C. The folowing illustration s the back of the instrument 1, mains switen 2 mains co ction (socket) has been set 3.1.2 Mains operation Attention! The mains voltage must coincide with the setting of the voltage selector. I he mains votage deviates a Conversion must be made. In order to do this the instrument, arated from the mains. 5 6 for 12 V battery ctor can be set Aller opening the cover the voltage s 10 100, 120, 220 and 240 V by turning up 10 90 MERCK 114 3.1.2 Mains operation << voltage selector <<. indicator pin When selecting the consumption of inlo account 3.1.4 Cell compartment The cell compartment permits the reception of 10, 20 and 50 mm rectangular cells, as well as rounc external diameter of 16 mm, without manual ac (insertion of adaptor ‘The positioning in the folowing, save wa cove ae MON 3.1.5 Keyboard he able membrane ke curity with its ing the of The w 3.1.5 Keyboard Nojclear (last result) Reverse cursor (eampio dilution) Parameter Forwards cursor (campie number) Funetion nter Decimal point (alpranumeric eymbo!) sign) I up the method list Call up the parameter lst ae Call up the function lst ¥ ° 4 Call up the blank value The decisions which appear in th 0.9, numbers or letiers are tran Determinations are set in motion play are confirmed, red to the memory. Line by line progression through the list wh been called up. Continuous pressure: run through of the list, Lower function: call up of the sample number Moving backwards line by line through the lst which has been called up. Continuous pressure: run through of, Lower function: call up of the sample dilution whi The de appear in the display are negated, for example, numoers or laters are erased, Lower function: display of the last result Decimal point Lower function: cal up of the alphanumeric symbol CAPM Start the timer MERCK 46 3.2 Carrying out an analysis ia if NERC K PHOTOMETER SQ 118 _U1.88 59 CT NITRATE NO3 14542 2.8 - 88.0 mg/l! 959 CT NITRATE NOS 14542 SELECTING FILTER 859 CT NITRATE NOS REACTION TINE > CLOCK @59 CT NITRATE NOS 90:08 REACTION TIME 19 + @ min i 959 CT NITRATE NO3 18:88 MEASURE BLANK @59 CT NITRATE NOS 18:03 8 ag/! @59 CT NITARTE NOS 18:86 NEASURE SAMPLE @59 CT NITRATE NOS 18:18 28.8 mg/l Switch on the instrument. The light will slowly warm up. 1.80 's the programme version. 059 —-Method number Nitrate Method name NOs Form inwhich results are given 14512 Articie number 2,0-80.0 Measuring range mgft Unit It another method is desired ‘enter the method numer a: search for the required number with [=] [=] When the method agpoars inthe isplay, press tne 67) key. Briet Gisplay. The fiter is belng made ready for operation, If reaction times are to be kept the timer can now be started. Continuous time display, When the reaction time is completed an acoustic signal bleeps. The time display ‘continues to run, For methods with 2 reaction times the second time is started by pressing the [0) key again, Insert cell with blank. Blank is being measured (zero adjustment, display 3 seconds) Insert cell with sample Result (display 3 soconds) MERCK 17 3.2.1 Lot factor By entering a lot factor the operator has the opportunity to correct minor chemically induced fluotuations and, thereby, obtain higher accuracy in the resull, The lot z factor isin the range 0.90 < FK s 1.10 and can be found fn the outside label of the Spectroquant packaging (for ‘most ceil tess). When opening a new package the lot factor must be checked and re-entered if necessary. desired concentration of the standard solution result on S118 Jo oe 859 CT NITRATE NOS 14542 2.6 - 68.8 ang/I 859 CT NITRATE NOS 14542 CELL 16 an 859 CT NITRATE NOS 14542 LoT FACTOR 1.88 059 CT NITRATE NO3 14542 SELECTING FILTER 59 CT NITRATE NOS 19942 2.8 - 68.8 ag/I 3.2.2 Series Determinations ‘As many series determinations as you ike can be carried ‘out against the same blank, ia ‘Afurther sample can always be measured when the reques Enter method. When the method appears in the display press (3) For this method the 16 mm round cell should be used. It the lot factor stated on the outside label of the package ciffers from that in the display the new lot factor must be entered, 8.9: (1) (+) (@) ©) Confirm entry. The lot factor is maintained until itis overwritten, even after ihe Insvument nas been shu om. ‘The lot factor is entered in the: calculation of the analysis result! Roturn to mothod. » MEASURE SAMPLE appecis. @59 CT NITRATE NOS 10:06 NEASURE SANPLE 059 CT NITRATE NO3 18:18 26.8 ag/l 959 CT NITRATE NO3 MEASURE SAMPLE 859 CT NITRATE NOD 16:16 45.8 ng/I 859 CT NITRATE NOS 18:21 NEASURE SAMPLE Insert next call with sample. Result (display 3 seconds) Insert next cell with sample. Result (cisplay 3 seconds) MERCK 118 3.2.3 Entry of a sample number to cusiomer, place where the sample The opportunity to enter an individual sample number data, e.g, accordi For exarnple: (identification number) enables suosequert sorting of the was obtained, € Sorting of date Customer Maller 7 | Le} Result Miler (Sample No. _007) determination sorting — in photometer ‘Customer Meier . according to Result Meier (Sample No. 81345) Sa118 cording it Meier in order of Gustomer Schafer your choice sample no. Cyne (Sample No. 391) bo Jo} Recut Sahater number (having a maximum of 6 digits) can always be entered after the request “MEASURE SAMPLE”. @59 CT NITRATE NOS sertoel wilt sample NEASURE SAMPLE 59 CT WiTANTC NOs 14542 SAMPLE NO. g8088 Bae lt you make a typing press (6), The exist be over All subsequent results will be saved and printed with this sample number. 059 CT NITRATE NOS Fee ered wl 20.8 ag/I povseved wih thi esul 3.2.4 Entry of a Dilution ror please .g number will fer the request ‘ofor the entry of the the sample has been diluted a dilution number can be The dilution number can be entered ered. For {urther Information about opti lluliun aid “MEASURE SAMPLE” or medial ‘on numiper see Section 1.2.3. sample number. 059 CT NITRATE NOS tesertcol wih sample NEASURE SAMPLE | 50 CT NITARTE NOS 14542 Enter dilution number, e.g. @) : In the case of a typing error erase SANPLE DILUTION 18 with (3). Orly whole numbers between 1 and 99 will be accepted Tre dilution number 's entered in ralewiation of the result! tis valid only for the sample which is now inserted. 59 CT NITRATE NOS 84.8 ag/I ab Result (display 3 seconds) Dilution number and sample number can be combined and entered in the order of your choice. MERCK 119 3.2.5 Last Result ‘The result appears in the display for 3 seconds and is then Changing the resuit-cisolay time is descrited in Section 3.4.9, saved, The resull-display timo of 3 seconds is an optimal The last result can be displayed a second time. Compromise between the time necessary 10 record the result and the rapid processing of series determinations, 859 CT NITRATE NOS NEASURE SAMPLE 950 GT NITRATE NOD “The last result is displayed again. 28.8 mg/l 3.2.6 Renewed Zero Adjustment When carrying out series determinations within a selected —_time. A renewed zero aciu method it iment cen be carried out at any practical to measure a fresh blank from lime 19 _time after the request "MEASURE SAMPLE”. Arrenewed zero adjustment is desired @59 CT NITRATE NOS after a measurement series. NEASURE SAMPLE $$) calep ot aro zero acs aso oT NITRATE NOS Insert col wih ftsh ban MEASURE BLANK 959 CT NITRATE NOD ‘The zero value appears in the display. & ng/l Insert call wth sample, 859 CT NITRATE NO3 MEASURE SAMPLE @59 CT NITRATE NOS Beicevay seccenss) 28.8 ng/I 3.2.7 Overview with all options The following diagram gives an overview of the operating sequence with all input possibilities, Basic operations and ‘options are distinguished by colour. The background for basic oporations Is dark grey. MERCK 3.2.7 Overview with all options Sohne — [ner muni wo all Call up different method G 7 (PORE ee mi Ch Call up brani: adjustment _ Ea} so [a For] bo) Rescrtan Tine — ova encanto] 8 An Switch on device Brit display Last method entered Search for a different method Required col! Wnecessary overwrite lot factor. ‘See package Brief display Briof display advice re: reaction time Start timer Reaction time running Ingert blank call Activate blank value adjustment Brief display blank value Insert sample cell Call up sample no, Itnecessary center sample no, Call up dilution necessary enter dilution Activate sample determination Briot dieptay. result MERCK 121 3.2.8 Result marking in the given measuring ranges of the layed. Resulis which le outside the measur- ing range marked with a x or not displayed at all Ifthe measuring values are 10% over the upper measuring range limit or between er0 and tne lower measuring range limit the result will be marked wih a x. These resulls could Indicate a larger measuring value error and should, therefore, only serve as orientati If the reaulte are moro than 10% over the upper measuring range limit the measuring range has clearly been exceeded, The results don't correspond t0 the real concentration. For this reason +4444 appears in the display. Nogative resuts, as can acour for example, ifthe blank and, ine sample solution have been mixed up, or alse with very small results close to zero, = appears in the display (exception: absorbance determinations) The folowing ilusiraivn clarifies resull marking using the ‘example of the nitrate determination method 59 Attention: dilution numbers which have been entered are taken into account. Tho result can, therefore, also be displayed correctly above the measuring range. 02 @59 CT NITRATE NO3 = ag/l 859 CT NITRATE NOS * 1,8 ag/! 859 CT NITRATE NOS 45.8 ng/I @59 CT NITRATE NO3 «85.8 mg/l @59 CT NITRATE NO3 teeter g/l 3.2.9 Calculation of results Fix-programmed methods are evaluated in different ways, |<—— measuring range —>| beet 80 88 mg/l NO; result negative rosult below the measuring range result within measuring range result above the measuring range result more than 10% ‘over the measuring range The type of evaluation is dependent on the shape of the ap DD A 4 cure 1 curve 2 | curves c c MERCK 3.2.9 Calculation of results Curve 4: linear relationship oxists between the absorbance and the concentration. The line runs through the z jon cue 1: C= AF ( Asal sation F = method’ dependent factor Curve 2: lino ie obtained wihich, however, doesn't run through the zero point. 3.3 Programming a method Programmi diferent ways: — With known factors, which, e.g. have been taken fro 1d data sheet or have been obtzined previously termination of a standard series. With standard solutions of known concentration. Curve 3: A nonlinear relationship, with a positive or negative vate, exists between the absorbance he concentration. Celeulation of curves 2 and 3: 4 abode curve parameters Caarb Asc Mad Ae ‘The number of decimal places is dependent on the formatting of the measuring range. Results are rounded up or down. All results calculations take ‘Tho input of the parameters specific to the method method Cat. no measuring rengo ell - wave i the same for both procedures. input of method parameters (1-7) with factors evauation t a near A enear factor enter curve parameter with standards ‘enter number and desired concen- trations of standara | determine standards ia MERCK 123 3.3.1 Evaluation with factors (ct) 2 \(0}(0) 200 METHOD UNDEFINED METHOD 81 METHOD NANE @1 METHOD NANE > HETHOD NAME >B- or HETHOD NAME >8: @1 METHOD WANE >BORON Ba~ @1 METHOD NANE “BORON B a2 CAT.NO a2 CAT.NO. 14938 03 NEASUAING RANGE Motnads 200-299 ara frraly programma Gonfirm the first letter Amaximum of 14 symbols can bi green sity. rose (= ones ‘The form in which the results are given (here B) is attached to the method name following a blank space. Taking on of the whole method name. Entry of the measuring range, w Maun f§ ait for weper and ower li ns eg ON OMI) — 63 NEASURING RANGE Ql - 2.5 MERCK 124 3.3.1 Evaluation with factors ww 4 UNIT a4 UNIT afl @5 REACTION TINE = tes min @5 REACTION TIME 4+ 0 ain a6 CELL yes 10 mm RECTANGLE 86 CELL wn 28 mm RECTANGLE @6 CELL YES 28 mm RECTANGLE ————— 87 WAVELENGTH yw 340 nn 87 WAVELENGTH yet 495 nm 07 WAVELENGTH ES 495 no @8 CALIBRATION WITH Y/N FACTOR FF @8 CALIBRATION WITH YES FACTOR —— 89 EVALUATION yw LINEAR 18 same as for with the keys 3) iaximum 7 pl method nur eg. al Entry of the eg. 00) 2 reaction timos Gan be entered (wnole numbers, max. 99 min.) Selection of the cell by repeatedly pressing the (2) key. Desired cel 20mm, Confirm cel! Selection of tho wavelength by repeatedly pressing the [) key Desired wavelength: 405 nm Confirm wavelength the cal Confirmation Selection of the evaluation. MERCK 125 3.3.1 Evaluation with factors 9 EVALUATION yes » LINEAR 10 FACTOR , Confirmation ofthe linear evaluation. tor, maximum of 28, €.9. 1.289 Confirm entry Return to method Fe Gl a Non-linear evaluation 89 EVALUATION VES LINERR 89 EVALUATIUN vn NON LINEAR @9 EVALUATION YES NON LINEAR 10 CURVE PARAMETER o 16 CURVE PARAMETER a.1942248 11 CURUE PARANETER b 14 CURUE PARAMETER © g 3 R For non-{inear evaluation (3) 's pressed, Change over to fon-iinear evaluation Move on to Enter curve paramet method data shest, €.9.0 Enter a minus with 've parameter a a fiom the 1940048 Contirm entry The further curve -d analogou entry with Return to method, 3.3.2 Evaluation with standard solutions Determination with known standards takes place according Programming a method (polygon procedure) to the polygon pracedure. The desired concentrations of tho standard solutions are entered and the SQ 118: absorbance ‘measures the corrosponding absorbances. Neighbouring measurng points aro connected by straight segments (polygon). The entire polygon group is saved in the SQ 118. ‘The evaluation of unknown samples takes place by linear interpolation between two measuring points. stondae 3 A fect ie ClewacFech concentration “The entry ofthe parameters 1-7 takes plac ‘ entra Same way a8 described in section 3.3.1. The [) key is pressed for @8 CALIBRATION WITH ¥/N ) Saiotantn wr Gancard FACTOR eee on ofthe cal “ @8 CALIBRATION WITH Y/N Selection of the calbraton STANDARD ‘ oo eRLISnATION WITH GEE) Selman cin caltatn STRHOARD try cf ruber of star ~ 1S WUNBER OF STANOAROS Ean = [Amaximum of 6 diffrent standards can be entered ee sfimation ofthe rumber ent > 15 NUNBER OF STANDARDS Confrmation of he sumer entry 6 ——————) _Eniryot the snecities concentration w 16 STANDARD 1 witha rraximum of places, 29. 0.3 s---- g/l — Confirmation othe number ent x

) artnor standards are entorec 17 STANDARD 2 ecenouh ween g/l Attention: Continuously confirm the 4 simbereries wi tne 003 hoy Move on with the [=] koy: The , standards can be éniered in any ord. ‘They are sorted according io size when 21 STANDARD 6 the method is called up. af (SID 1 MEASURING RANGE" will appear and the incorrect standard is dsplayes. MERCK 129 3.4 Description of the functions All data having precedence over methods and the service functions are in the function list. Of the 28 functions some serve data documentation and are used frequently e.g. result printout (function 1), others are used infrequent, e.9. time (Function 11) for the changeover from summer to winter time, ‘or are only set once by the user, ¢.g. the language (function 12). The service functions 20-28 are exclusively Used by the aftersales service Direct call up of a function: (A) @) GI Search for a function: (5) (=) [=] Attention: the cursor does not appear in the upper left hand ‘comer of the display after pressing the [= key, ‘the key should be pressed again. When the (EI) key is pressed the function which was last selected will always be shown, (Many comments are treated as a question (YIN) which is atfrmed by pressing the (1) key or negated by pressing the C3) key, 3.4.1 Printing out results ‘The printout of results takes place with a customary printer, The results can be sorted according to three different criteria Fuserron List PAINT AES! OUsPLay RESULTS RESULTS To conuren ConsecurcuE. No PRINT neTHOO List PRINT PRABMETER LIST PRINT FUNCTION LIST FoRnreee. RESULT DISPLAY Tine 3 sevunus bare 23-82-95 Tine 1501923 Lancuase ENGLISH Auranatic neAsusenent EUERY 1@ seconDS futanetie nensunenent ENABLE cy ConpUTER IATER=aCE onra"gits.t COMPUTER INTERFACE S10? B1Ts 2 COMPUTER INTERFACE PARITY EUEN COMPUTER IATERFACE DELAY a3ee es CORPUTER CHECK Disecay cxece PRINTER CHECE FILTER ROTOR CHECK FILTER CaECK TER CHECK 1 TER GuERE > cheek Svsten ‘all methods in the order the determinations were made ‘* methods sorted with or without parameter printout ‘ sorted according to sample number Result printout: all methods: 1 PRINT RESULTS 81 PRINT RESULTS FROM 31,085.95 @1 PRINT RESULTS ALL METHODS @1 PRINT RESULTS PLEASE HAIT dd doo Call up of result printout Search for or enter the date of the desired determinations with the (=) key. Te esults of al the methoos termined should be printed out yen * Brief display. MERCK 131 3.4.1 Printing out results RESULTS OF 31,05,95 HeTHOD Tine No RESULT/UNIT SAMPLE NO 926 ANNONIUN NHS taa2 8.5 mg/i Wd 14 629 ci co 1:85 2 224 na/l 14 29 cr Coo Wiz 3 358 ma/t 209 929 cT coo 18 4 1288 mast 3587 — 834 IROH Fe 11:34 5 * 8.2 mnol/ad Fe | 14 | 834 IRON Fe iy 6 $.7 mnol/n3 Fe 269 = 934 IRON Fe 1487 15.8 mmol /n3 Fe 3587 — age AMMONIUM HH4 11:52 8 3.2 ag/i WHA 209 886 ANNONIUN NHE 11:56 9 teeeee mg/l WH4 = 3587 -. swering this question using FORNFEEO key or the FC) sey the Y/N display "ALL METHODS" reappears. Printout of results sorted according to methods PRINT RESULTS seagate eee ALL METHODS van a1 PRINT RESULTS This question is affirmed SORT METHODS wi ‘Tho parameters measuring PRINT RESULTS range, cell, wavelength, jot factor PRINT PARAMETER wen and article number will be printed ‘ut a5 wel. not desired press the (2) key Last metnod used in memory @1 PRINT RESULTS The desired method can be g96 AMMONIUM NH4 searched for with the (=) key, or the desired method number can be entered, 6.9. (8) All results and the parameters of the PRINT RESULTS Solected method willbe printed out PLEASE WAIT i oj oe RESULTS FROM 91.05.95 HETHOD TIME NO. RESULT/UNIT SAMPLE HO ag6 ANNONIUN NHS 18:92 OS mg/l HA 14 886 AMMONIUM NH# 11:52 8 3.2 ug/l NH4 289. 886 ANNONIUN NHS 11:56 9 t4eeee mg/l NH | 9587 Aor answering this question with (©) FORNFEED. the next method appears automaticaly Y/N in the display. MERCK 132 3.4.1 Printing out results Result printout sorted according to sample no. PRINT RESULTS ‘Answer question in the negative. ALL METHODS vn Answer question in the negative Qi PRINT RESULTS SORT METHODS wn PRIN RESULTS This question is atfirmed, SORT SANPLE NO. yen The sample number last entered 1 PRINT RESULTS ‘appears in the cisplay. Search for SANPLE NO. 289 the desired sample number with the [=} key or enter as number, eu. DOE) PRINT RESULTS PLEASE HAIT ij daw RESULTS FROM 31.95.95 neTHOo TIME NO. RESULT/UNIT SAMPLE NO. aos anmonrun we 11:52 8 ~~ ~3,2 ag/1-NMY 209 9 cr coo tz 3388 g/t 269 054 inoW Fe Hike 8 SNF Bkotvas re 269 ‘Aor answering this question with FORNFEED the (a) x9y oho.) key the next wun Sample number appears a.roratally inthe dspiay MERCK 133 3.4.1 Printing out results @ ec) OF PRINT REBUCTE (ar BE =) search for desired date aon 22.08.05 Overview of the result printout largely applies also to Function 2: display results Function 3: results to computer Bu nesneoe ws Soet neTHOES SenbLe nor SORTED ye J i search for desired I semen, eS be [rare va rami vn amare — ——t— fo) fo) fo) ) i 2 J T MERCK 134 3.4.2 Displaying results All results which have been saved can be displayed ‘The operation takes place in a similar fashion to individually and called up according to three different described for function 1 result printout sort criteria: ‘all methods in the orcier the dinterminations ware made * sorted according to method ted according to sample number. Callup the display results, @2 DISPLAY RESULTS Search for the date of th > 82 DISPLAY RESULTS desired determination o FROM 31,85.95 enter with the (=) Key. I All methods should be displayed. 82 DISPLAY RESULTS » ALL METHODS wa > 306 anmonTun Wie 14 Depiay othe tsreout a 182 ethod qumber 8.58 ag/! 1818 Ammonium — method NH form in which the resut given 4 sample nurbe 1 consecutive number 050 resu 10.02 ime of the determination — yap er coo Move on tothe next By repeated pressing of te [ 2 224 mg/l 11,85 all of the results will be displayed ‘ne after the other. + caling up al of the resuts 02 DISPLAY RESULTS After calling up al of the res ALL METHODS ¥ the cleplay "ALL. METHODS" MERCK 435 3.4.3 Transferring results to a computer The resulis can be transferred to a computer according to _The operation takes place analogously to function three different sort criteria: result printout ‘all methods in the order the determination were made ‘sorted according to method ‘* sorled accoraing to sample number. @3 RESULTS TO COMPUTER 83 RESULTS TO COMPUTER FRO 31.85.95 83 RESULTS TO COMPUTER ALL METHODS wn 09 RESULTS TO COMPUTER PLEASE HAIT ddodoeo @3 RESULTS TO COMPUTER ALL METHODS vst 3.4.4 Setting of a consecutive number 84 CONSECUTIVE NO. aat Call up of function 3. ‘Search for the date of the desired determination with the [=) key or enter ‘All methods should be transferred to the computer Brief display. Alter tenemission of the data "ALL METHODS" reappears in the display. The consecutive number is auto- matically set to 1 ater the first ‘switching on following a change of date. Itruns up to 999 and then begins, again with 1. By entering a3 figure number the runing number can be ataried at any point, 0.4. for corios determinations. 3.4.5 Printing out the method list ao 85 PRINT METHOD LIST The method ts out in three ways: * all methods * tree methods + fixed methods 2 rintout of all methods. a OS PHINI MEIHUU LIST ALL METHODS wn @5 PRINT METHOD LIST PLEASE WAIT |All methods should be printed out, (out of @ complete method fist ‘oliows (se0 section 1.1.4). Printout of the freely progra 85 PRINT METHOD LIST mmed methods and the free method storage space his question is answered in the negative. ALL METHODS wn Confirmation vith tho CED key. “ 5 PRINT NETHOO LIST FREE NETHODS ves oo riniout of te hroely prgrarnmed 9S PRINT METHOD LTST methods and the free metrod » PLEASE WAIT Printout of the fixcprogrammed Merck methods - @5 PRINT METHOD LIST tendo, were in ALL METHODS 7) pi 05 PRINT HETHOD LIST TOS eelgn S enewerea in FREE METHODS wn onfrmation the printout 4 85 PRINT METHOD LIST of te fhe orogrammed Mele FIX METHODS wan methods follows ot ciopi @5 PRINT METHOD LIST Brot clspley » PLEASE MAIT MERCK 137 3.4.6 Printing out the parameter list (—){s) Co) PARAMETER LIST 1 METHOD Nane 22 cAT. to 83 NEASURING RANGE 4 UNIT 85 REACTION TIME 6 CELL 7 WAUELENOTH 88 CALIBRATION 89 EVALUATION 18 FACTOR 6 PRINT PARAMETER LIST METHOD NO IRON Fe 14761 8.2- 2.5 g/l Fe 3'+ @ minutes 28 am RECTANGULAR 50s nm ITH FACTOR LINEAR 1,899 3.4.7 Printing out the function list (C) Q? PRINT FUNCTION LIST 3.4.8 To start the formfeed on the printer (I) Cm) ge FORMFEED 3.4.9 Setting the result display time (I) (9) Cm) 09 RESULT DISPLAY TINE 83 SECONDS Printout of the parameter list Of the mothod last selected, Printout of the complete function ist (see section 3.4) Effocts moving on by one page ona printer. Con tothe ‘orm food Key of printer of 1-9 seconds, oe appear in tho display for 3 seconds. The instrument is delivered with this pre-set optimized tim MEKCK 138 3.4.10 Setting the date, time and language (0) Once the date has been entered 18 /DRTE eg HO O8 BS lal 16,06.95 the calendar cor ‘torur automaticaly After entering the tie, 11 TIME 3) Oo) 26. 08 0 BO 12:37:08 tho clock rune in 24 hour operation Call up of the language. Tr 12 SPRACHE repeated pressing of the [) DEUTSCH JA German, English, French, Htalian, Spanish, Finnish, Danish, Swedish, Indonesian, Polish, Portug Hungarian, Turkish, Czech and uutch can be selected. 12 LANGUAGE ENGLISH yen Confirm, 6.g. English. 12 LANGUAGE ENGLISH, yes Hd ove de MERCK 139 3.4.11 Automatic measurement Periodical determinations in intervals of 10-99 seconds are possible with functions 13 and 14. Application exemple: flow through determinations, reactions dependent on time, etc. 13 AUTOMATIC MEASUREMENT eg. [2] (0) Pol. 13 AUTOMATIC MEASUREMENT EVERY 20 SECONDS ove onto function 14 and switch 14 AUTOMATIC MEASUREMENT Sreuapmetie dotorrinetion wah FHARIE NA ‘ho bea) “ey —— w be callod up, to) Te aUTOTATIO HERSURENENT cue ceo ip ves Absorbance 248 ABSORBANCE 8.008 - 3.008 A 249 ABSORBANCE SELECTING FILTER ——e—e—e—e—e—eee ST 249 ABSORBANCE = ——~—~Y)~S«CS= DN NEASURE BLANK Sa) Blank is measured (zero adjustment) 248 ABSORBANCE Insert sample solution, 8.080 A 248 ABSORBANCE Fee rome iekes place. AUT, MEASURE EVERY 20 SEC ‘hiss stopped by pressing the (Gi) key. This results in parameter ‘4 “AUTOMATIC MEASUREMENT" being set to "NO" MERCK +40 3.4.12 Computer connection ‘ons 15-20 the interface to the computer can he format for transmission ation see section 35.2 EG 15 COMPUTER INTERFACE » BAUORATE 9600 yes > 15 COMPUTER INTERFACE LJ BRUDRATE 2400 ves 1& PANPIITFR INTERFACE DATA BITS 7 YES Te COMPUTER INTERFACE 17 COMPUTER INTERFHLE 17 COMPUTER INTERFACE ld STOP BITS 2 ves > 16 COMPUTER INTERFACE PARITY OOD YES 16 COMPUTER INTERFACE » PARITY EVEN ves » DATA BITS 8 ves C—) DATA BETS BES » STOP BITS 1 YES EC) Step BITS | SES) Possible seiting of the baud rate: 9600, 4800, 2400, 1200, 600, 300. Setting of another baud rate throug repeatedly pressing the (LI) key, e.g. 2400, Confirmation of the input Confirmation of the input. Possible getting ofthe stop bits: Vor 2. Chai with the (13) key. CContirmation oft Io setting of the party NO, ODD, EVEN. the [EC key. Confirmation of the input. 3.4.12 Computer connection do ooo (9) 19 COMPUTER INTERFACE DELRY ---- as 19 COMPUTER INTERFACE DELAY 0308 me 28 COMPUTER CHECK Vi The delay time between the sending of two data blocks can be set yeen 10 and 9990, eg FOO Checking the interface tothe computer, MERCK 442 3.4.13 Service functions i 21 KEYBOARD CHECK (ws) 22 DISPLAY CHECK (o) 23 PRINTER CHECK (s) 24 FILTER ROTOR CHECK » 24 FILTER ROTOR CHECK » TUANTHG FILTER ROTOR 25 FILTER CHECK Service function for testing the keyboard. Tre current meaning of the key in the display appears by pressing the key. Interrupt by pressing the (C3) key. Service function for testing the display. All possible symbols brought tothe display. Intern pressing the (C2) key ty Service function for testing the printer. Tha entre symbo! store ofthe printer is printed out interrupt by pressing the (<] key. ‘Service function for checking the ‘easy operation of the filter rotor. Interrupt by pressing the (3) key. Service function for checking the > filter. ach fits piacee in beam path anc measured > 25 FILTER CHECK Bret cisely SELECTING FILTER FSET) Esto all a zero adstnent with 25 FILTER CHECK the 625 nm fiter is made. AIT filters FILTER 635 nm = 8.080 A} — aremeasured against this fiter and "the current absorbance displayed. Attention: I printer is connected the resuits will only be pimog out Tho conice functions 26-28 are ox forthe and not displayed Use ofthe speciaized custorne production the final chook. These functions cannot be meaningfully activated by the user. MERCK 143 3.4.14 Function structure 144 3.5 Appendix 3.5.1 Printer connection The SQ 118 photometer has an 8 bit parallel centronics interface. Tre connector assignment of the 26 pole socket ig identical to the IBM AT Personal Computer socket. Data can be output with the interface mentioned ‘above with a printer cable to a cusiomary printer Attention: When installing, putting into operation and setting the printer, in particular the DIP switch, alease consult ‘the operating handbook for the printer. FORNFEED wn 1 during data transmission to a printer ched on 1 Ue printer is nt in the "ON LINC mee or ‘© the printer is not swt ‘+ the printer cable between the photometer ‘and the printer is loose the following message appears PRINTER NOT READY # ‘The printer cable must be firmly connected between the photometer and the printer. © “The printer must be "ONLINE" curing deta communication. * A suitable standard print should be chosen. ‘Attention: If proportional print is chosen the umber and letter colurnns are not exactly aligned when printed out ‘© Paging Is controlled through the keyboard of the paotometer The (5) key effects moving the paper lorward by 1 page. ‘The (2) key moves the paper forward by 5 lines. The result printout follows resurmption of the "ON LINE" connection and ABORT FUNCTION ¥/H pressing ofthe (C3) key Pressing the [ 6 al 200-1500 nm Photometric A> 2at 340nen measuring range: ‘> 3 at 405-820 1m with reference to distiled water <05%atA=1 Accuracy: 1% atA=t Photometric resolution: A=0001 ‘Warming up time: <5 minutos Photometer drift: .01/h alter warming up time Measuring time: < 35 Types of determination: concentration, absorbance, transmission Zero adjustment: sutormatic al the press of a key ‘Methods: 190 methods fix-programmed 80 methods freely programmable Result memory: 250 results, shift register, can be called Up eccording to aiferont ortoria Unit conventional (mg/) or SI (mole) Keyboard: rmaisture-proo, 20 keys with tactile feedback Display: 2x24 digit LCD cieplay with large angular display area 3.5.6 Delivery programme Delivery programme Cat No. 14720: Photometer SO 118 in carrying case complete with instruction manual, replace ment lamp, fuses, dust cover, 12 volt DC connection cable and screw driver, ‘To obtain spare parts and for service questions please contact INSTRUMENT-SERVICE MERCK. user dialogue with logical user guidance in 19 languages (German, English, French, liaian, Spanish, Danish, Swedish, Finnish, Indonesian, Polish, Portuguese, Hungarian, Turkish, Czech and Dutch) User guidance: Cells: cell compariment for: 10mm rectangular cols, min. full vol. 4 i 26 mm rectangular cells, min. full vol. 2m! 50 i vecten ular cells, mir. full vol & mt 46mm round cols, "min. full vol. 3m 100, 120, 220, 240V-AC + 20/~ 10%, changeable, 60, 60 Hz, + 5%, 12 V-DC ‘connection fer operation witn car battery Power supply: Power input: 20VA, 10-35°C for defined precision and accuracy 0-80°C for broader precision and accuracy 0-70°C outside work 25-70% ralative humicity, not drop protect from direct sunlight Environmental conditions: Centronics parallel interiace for printer (25 pol. SUB MIND socket) compatibie vwith IBM, All printore with this intertaco can be connected. Printing format 80 strokestine ‘Computor- connection: = 24 RS 252 interface Calibration: For trooly programmable methods with slandards automatic curve adjustment with polygon group. Time Integrated calendar, recording of real measurement: {ire with date and time, can be called up, integrated timer Standards and in accordance with VDE, SEV, regulations: High frequency law, GS Dimensions: length 290 mm width 230 mm height 400 mn Weight: 35 kg Accessories: Cat No. 14946: Rectangular cells, 10 mm (1 pack with 2 celis) Cat.No. 14947; Rectangular cel's, 20 mm (1 pack with 2 cells) Cat.No, 14944: Rectangular cel’s, 50 mm (1 pack with 2 cells) Cat.No, 14724: Round cells with screw caps, 16 mn (25 pioces) Cat.No, 14902: Flat-bottomed tubes with screw caps. (12 pieces) Cat.No, 14728: Halogen lamp for SQ 118 MERCK 148 Merck KGaA, Frankfurter StraBe 250, D-64271 Darmstadt, Tel. (06151) 720 pvr zn srt60098

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