SQ NOVA 60 Manual - en - 2012 - 01
SQ NOVA 60 Manual - en - 2012 - 01
SQ NOVA 60 Manual - en - 2012 - 01
Operating manual
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Operating manual
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General Information
Spectroquant photometers
Contents
1 Photometers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1.1 1.2 Photometry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . The Photometers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 5 6 6 6 7 7 8 8 10 10 10 11 11 12
2.2
3 Sample Preparation. . . . . . . . . . . . . . . . . . . . . . . . . . 12
3.1 3.2 3.3 3.4 3.5 3.6 Taking Samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Preliminary Tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Dilution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Filtration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Homogenization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Decomposition . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 13 13 14 15 15
5.3 5.4
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1 Photometers
1.1 Photometry
When a beam of light is transmitted through a colored solution, then this beam loses its intensity, in other words a part of the light is absorbed by the solution. Depending on the substance in question, this absorption occurs at specific wavelengths. Monochromators (e. g. narrow-band interference filters, lattices) are used to select the wavelength from the total spectrum of a tungsten-halogen lamp (VIS spectrum), a deuterium lamp (UV spectrum) or, respectively, a xenon lamp. The intensity of the absorption can be characterized using the transmittance T (or, respectively, T in percent). T = I/I 0 I 0 = Initial intensity of the light I = Intensity of the transmitted light If the light is not absorbed at all by a solution, then this solution has a transmittance of 100 %; a complete absorption of the light in the solution means 0 % transmittance. The measure generally used for the absorption of light is the absorbance (A), since this correlates directly with the concentration of the absorbing substance. The following connection exists between absorbance and transmittance: A = log T Experiments by BOUGUER (16981758) and LAMBERT (17281777) showed that the absorbance is dependent on the thickness of the absorbing layer of the cell used. The relationship between the absorbance and the concentration of the analyte in question was discovered by BEER (18251863). The combination of these two natural laws led to the derivation of Lambert-Beers law, which can be described in the form of the following equation: A=
c d
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1 Photometers
1.2 The Photometers
The photometers that belong to the Spectroquant Analysis System differ from conventional photometers in the following important aspects:
The calibration functions of all test kits are electronically stored. The measurement value can be immediately read off from the display in the desired form. The method for the test kits (Cell Tests and reagent tests) belonging to the Spectroquant analysis system is automatically selected via the scanning of the bar code. All cells formats used are automatically identified and the correct measuring range is selected automatically. Instrument-supported AQA ensures that measurement results can be used as secure, reproducible, and recognized analytical results. New methods can be downloaded from the internet site www.merck-chemicals.com/photometry and permanently stored in the instrument.
For technical data and instructions for use please refer to the section Function description or can also be found on the internet.
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Identification mark for the correct insertion into the cell compartment of the photometer Cat. No. of test kit Designation of test kit Details regarding contents Special cell in optical quality
14560 CSB/COD
Quecksilber(II)-sulfat, Schwefelsure Mercury(II) sulfate, sulfuric acid Mercure(II) sulfate, acide sulfurique Mercurio(II) sulfato, cido sulfrico
Leakproof cap Bar code for identification in the photometer Risk phrases Highly precise dosage of the reagent
Additional reagent(s) Certain cell tests, e. g. COD or nitrite, already contain all necessary reagents in the cells, and the sample must merely be added with a pipette. In other tests, however for reasons of chemical compatibility it is necessary to separate the test into two or three different reagent mixtures. In such cases, besides the sample a metered reagent must also be added.
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Absorbance
Concentration
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114739 114558 114544 114559 114752 100683 100605 100595 100597 100598 100602 100599 100086/ 87/88 100608 114553 114767 114557 100809 114598 100606 101632 100607 114551 114831
Ammonium CT Ammonium CT Ammonium CT Ammonium CT Ammonium Test Ammonium Test Bromine Test Chlorine CT Chlorine CT Chlorine Test Chlorine Test Chlorine Test Chlorine Test Chlorine Dioxide Test Copper CT Copper Test Fluoride CT Fluoride CT Fluoride Test Iodine Test Monochloramine Test Ozone Test Phenol CT Silver Test
turquoise instead of green turquoise instead of green turquoise instead of green turquoise instead of green turquoise instead of green turquoise instead of green yellow instead of red yellow instead of red yellow instead of red yellow instead of red yellow instead of red yellow instead of red yellow instead of red yellow instead of red turquoise instead of blue turquoise instead of blue brown instead of violet brown instead of violet brown instead of violet yellow instead of red turquoise instead of green yellow instead of red weakening of color no change (flocculation)
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10
20 30 Temperature (C)
40
60
10
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raise the measurement value as a result of an amplification of the reaction lower the measurement value as a result of a prevention of the reaction.
A quantification of this effects is stated in tabular form in the respective package inserts for the most important foreign ions. The tolerance limits have been determined for the individual ions; they may not be evaluated cumulatively. Suitability for use in seawater A tabular survey (see appendix 1) provides information on the suitability of the tests in connection with seawater and also on the tolerances for salt concentrations.
A positive-displacement pipette should be used for larger quantities of liquid or for the exact dosage of smaller reagent quantities. In these cases the reagent bottles are not fitted with a dropper insert.
Solid substances are dosed either with the dose-metering cap or with microspoons that are integrated into the screw cap of the respective reagent bottle. The dose-metering cap is used for solid reagents or reagent mixtures that are free-flowing. In all other cases the substances are dosed with the microspoon. In this case it is necessary to add only level microspoonfuls. To this end the spoon must be drawn over the brim of the reagent bottle.
At the first use replace the black screw cap of the reagent bottle by the dose-metering cap. Hold the reagent bottle vertically and, at each dosage, press the slide all the way into the dose-metering cap. Before each dosage ensure that the slide is completely retracted. Reclose the reagent bottle with the black screw cap at the end of the measurement series, since the function of the reagent is impaired by the absorption of atmospheric moisture.
m
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3 Sample Preparation
Sample preparation covers all the steps necessary before the actual analysis can be performed.
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3 Sample Preparation
3.2 Preliminary Tests
Correct measurement results can be obtained only within the measuring range specified for each individual parameter. When dealing with sample solutions of an unknown concentration, it is advisable to establish whether the sample concentration is indeed within the specified measuring range, ideally roughly in the middle of the range. Preliminary tests enhance the analytical reliability and make the determination of the necessary dilution ratios in the case of high concentrations easier. Merckoquant Test Strips are very well suited for preliminary tests.
3.3 Dilution
Dilution of samples is necessary for two reasons:
The concentration of the parameter under investigation is too high, i. e. it lies outside the measuring range. Other substances contained in the sample interfere with the determination (matrix interference); false-high or false-low results may ensue.
The following auxiliaries are absolute prerequisites for the dilution of the sample: Volumetric flasks of varying sizes (e.g. 50, 100 and 200 ml) Positive-displacement pipette Distilled or DI water.
Only dilutions carried out with these auxiliary products are of sufficient reliability in the area of trace analysis, to which photometry belongs (for the simplified procedure see page 14). An important aspect here is that once the volumetric flask has been filled up to the mark with distilled water the flask is closed and the contents are thoroughly mixed. The dilution factor (DF) resulting from the dilution procedure is calculated as follows: Final volume (total volume) DF = Initial volume (sample volume) The analytical result is subsequently multiplied by the dilution factor. A calculation can be dispensed with when the dilution is programmed into the photometer. The dilution number (see the table on page 14) is entered and the measurement value is subsequently calculated correctly and immediately displayed.
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3 Sample Preparation
All dilutions should be made in such a way that the measurement value lies in the middle of the measuring range. As a rule, the dilution factor should never be higher than 100. In the event that yet higher dilutions become necessary all the same, then this must be done in two separate steps. Example Step 1: Step 2: Make up 2 ml of sample to 200 ml with distilled water; DF = 100, dilution number 1+ 99 Take 5 ml of the above solution and make up to 100 ml; DF = 20, dilution number 1+19
The dilution factor for the total dilution is calculated by multiplying the individual dilutions: DF total = DF1 x DF2 = 100 x 20 = 2000, dilution number 1+1999 Simplified procedure Dilutions up to 1:10 can also be prepared without volumetric flasks in a glass beaker, measuring the volumes of the sample and the dilution water using a previously calibrated positive-displacement pipette (see table for instructions).
Desired dilution Volume of sample [ml] Volume of distilled water [ml] Dilution factor Dilution number
5 5 2 2 1
5 10 6 8 9
2 3 4 5 10
3.4 Filtration
Strongly turbid samples require pretreatment before they can determined in a photometer, since the effect of turbidity can result in considerable variations in the measurement values and in false-high readings. Care must be taken here to ensure that the substance to be determined is not contained in the suspended material, in which case a sample decomposition must be carried out. Compounds that always occur in dissolved form (for example ammonium, nitrate, nitrite, chlorine, chloride, cyanide, fluoride, orthophosphate, and sulfate) permit a previous filtration, even when the sample solution is strongly turbid. Weak turbidity is eliminated by the automatic turbidity-correction feature built into the photometer (see Function description, Device set-up/ Correction function); in such cases it is not necessary to filter the sample before analysis. As a measure to distinguish between dissolved and undissolved waterborne substances, the water sample can be filtered through a simple paper filter. Following the recommendations stated in the reference methods, membrane filters with a pore size of 0.45 m are required for fine filtration.
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3 Sample Preparation
Procedure for microfiltration
Screw the syringe tightly into the front side of the membrane-filter attachment.
Hold the syringe upright and slowly depress the piston upwards until the membrane- filter is fully wetted free of air bubbles.
Filter the contents of the syringe into the intended glass vessel.
3.5 Homogenization
As a measure to ensure that a representative sample can be taken in the presence of suspended matter in the water sample in question, for certain parameters - e. g. COD and the total content of heavy metals - the sample must be homogenized. This must be carried out using a high-speed blender (2 minutes at 5000 20 000 rpm and taking the sample while stirring.
3.6 Decomposition
Ion
Water-borne substances can be present in the sample for investigation in a variety of forms: as the ion, bound more or less solidly in a complex, or as a solid substance.
Complex
Solid substance
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3 Sample Preparation
The manner in which the sample is pretreated enables the three proportions to be distinguished from each other. This can be illustrated using a copper-containing wastewater sample as an example. Example
Total content Dissolved proportion Dissolved proportion Solid Substances Cu(OH) 2 Complexes Cu-EDTA Complexes Cu-EDTA Ions Cu 2+ Ions Cu 2+ Ions Cu 2+ Result A Proportion: Ionogenic Complex Solid Substances Total content Result B Result C
=C = BC = AB =A
Decomposition converts the substance to be determined into an analyzable form. In most cases, decomposition agents take the form of acids in combination with oxidizing agents; in exceptional cases (e. g. in the determination of total nitrogen) an alkaline decomposition is more effective. The type of decomposition procedure used depends on the analyte to be determined and the sample matrix.
The ready-to-use sample-decomposition products Spectroquant Crack Set 10 and 20 are suited for the preparation of the sample materials for the determinations stated in the table. The decomposition processes are carried out in the Spectroquant thermoreactor (capacity: 12 or 24 decomposition cells) at 120 C or, respectively, 100 C. Details regarding the heating times and further treatment can be found in the package inserts contained in the Spectroquant Crack Set packs.
Determination of Total phosphorus* Total chromium* [= sum of chromate and chromium(III)] Total metal [= sum of free and complex-bound metal] Total nitrogen*
Sample preparation with Crack Set 10 / 10C** Crack Set 10 / 10C Crack Set 10 / 10C Crack Set 20
* The decomposition reagents are already contained in the packs of the respective cell tests. ** Decomposition cells are included in the pack; empty cells are required for the decomposition for Crack Sets 10 and 20.
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3 Sample Preparation
In the event that the sample to be analyzed is a highly contaminated material (high proportion of organic substances) or water-insoluble samples, decomposition using concentrated acids and other agents is indispensible. Corresponding examples from the collection of applications for real samples are available on request. The necessity for decomposition can be checked according to the following diagram: Decomposition Procedure Measurement Result A Procedure Measurement Result B
Decomposition necessary
No
A and B idential?
Yes
No decomposition necessary
For wastewater with a consistent composition, this check as a rule need be carried out only once. It is, however, advisable to check the result periodically.
4 Pipetting System
Positive-displacement pipettes permit
an exact dosage of the sample volume a precise measurement of sample and reagent volumes and of the volumes of water for dilution purposes.
Pipettes of varying volumes and also ones with a fixed volume are available. Sources of error and hints on how to avoid them:
Closely follow the instructions for use contained with the pipette in question. Check the pipetted volumes a) by weighing using analytical scales (weighing accuracy 1 mg), 1 ml of water at 20 C = 1.000 g 1 mg b) using Spectroquant PipeCheck; this is a photometric check of the pipette, and scales are not necessary (see section AQA).
Avoidance of spread effects by rinsing the pipette several times with the solution to be pipetted. Always exchange the pipette tip. Draw up the liquid slowly and depress piston completely to discharge the liquid.
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the working materials used the handling the sample under investigation.
These errors have effects on both the accuracy and precision of the results obtained.
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The certificate for the test kit, available for each lot produced, documents the quality of the reagents contained in the test kit. Calibration function: The calculated function must agree, within specified tolerances, with the function electronically stored in the photometer. Confidence interval: Maximum deviation from the desired value over the entire measuring range; every measurement value can be affected by this deviation; this parameter is a measure for the accuracy. Standard deviation for the procedure: Measurement for the dispersion of the measurement values over the entire measuring range, expressed in mg/l.
Charge-Nr. / Lot no. / Lote nro. Verwendbarkeit Expiry date / Fecha de caducidad Standard / Standard / Patrn Photometer / Photometer / Fotmetro Wellenlnge / Wavelength / Longitud de onda Kvette / Cell / Cubeta Prfer / Tester / Verificador Datum / Date / Fecha Datei / File / Fichero
HC119527 31.10.2012 Potassium hydrogen phthalate 1.02400 Referenz / Reference / Referencia 340 nm 16 mm rund / round / redonda Fr. Brandner 20.09.2011 1145600001_HC119527_EN
Kalibrierfunktion / Calibration Function / Funcin de calibracin DIN 38402 A51 / ISO 8466-1 Steigung / Slope / Pendiente +/- Tolerance / Tolerancia Ordinatenabschnitt / Ordinate segment / Intersecto en ordenadas Reag.blindwert / Reagent blank / Valor en blanco del react +/- Tolerance / Tolerancia Vertrauensbereich (95% Wahrscheinlichkeit) Confidential interval (P=95%) / Intervalo de confianza (95 % de probabilidad) Verfahrensstandardabweichung Standard Deviation of the Method / Desviacin estndar del procedimiento Verfahrensvariationskoeffizient Variation Coefficient of the Method / Coeficiente de variacin del procedimiento