Introduction. Thank you for your purchase of the Persee Analytics Inc. T8DS spectrophotometer.

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2 Introduction Thank you for your purchase of the Persee Analytics Inc. T8DS spectrophotometer. UV-Visible Spectrophotometer analysis is a well-accepted, documented technique with many applications. The technique is extensively used for the analysis of agricultural products, public health, environmental protection, life science industries and many other organic and biochemical applications. For obtaining maximum performance and trouble-free operation, please see the following suggestions: Upon receiving your instrument, please check that all the items listed in the packing list are included and install the instrument according to the instruction manual. The spectrophotometer is a precise electronic instrument. Please read the instruction manual carefully before operation. If the equipment is used in a manner not specified by the manufacturer, the protection provided by the equipment may be impaired. Avoid impact and handle the instrument carefully during transportation. If the tested solution is harmful to humans, please wear gloves or use other protection methods. Please keep the accessories in a safe place for the use in future maintenance. For more information, please visit

3 Contents Contents... I Chapter 1 Instrument Introduction Components inspection UV/Vis spectrophotometer and method UV/Vis spectrophotometer method UV/Vis spectrophotometer Condition of measure method Components description Front view Rear view Side view Sample cell holder Specifications... 6 Chapter 2 Installation Installation location Installation Start Installation performance The accuracy and reproducibility of wavelength Flatness of the baseline Chapter 3 Instrument operation About double beam measurement What is double beam How to use a double beam instrument Application examples Photometric measurement example Spectrum measurement example Quantitative measurement example Chapter 4 Optional accessories CH19-1 Thermostatic cell holder DS19-1 Angle-changeable solid sample holder IS19-1 Integrating sphere LS19-1 Long pathlength cell holder MH19-1 Micro cell holder MH19-2 Ultra-micro cell holder MR19 1 Specular reflection accessory MS19-1 Manual 8-cell holder PS19-2 Sipper pump S19-1 Solid sample holder SS19-1 Short pathlength cell holder... 33

4 4.12 TR19-1 Test tube cell holder Chapter 5 Maintenance Points for attention: Daily care Trouble shooting and maintenance Appendix 1 Light source replacement Replace the tungsten lamp Replace the Deuterium lamp Appendix 2 Fuse replacement... 44

5 Chapter 1 Instrument Introduction 1.1 Components inspection After the instrument has been unpacked, please check carefully all the parts provided against the packing list. In the event of error or damage, contact your local sales agent immediately. A complete set with the instrument according to the packing list should be supplied. The company keeps the right to revise the packing list. 1.2 UV/Vis spectrophotometer and method UV/Vis spectrophotometer method A UV/Vis spectrophotometer instrument analysis method measures the molecular absorbance of radiation in ultraviolet and visible spectrum. The absorption of the molecules corresponds to the excitation of valence electrons and electrons in the molecular orbital between different electronic energy levels. The analysis methods can be used for quantitative analysis of organic and inorganic compounds. Lambert-Beer s law is the basic law of radiation absorbance; it is the foundation of spectrophotometer analysis methods. The absorbance (A) of a solution is directly proportional to the path length (b) and the concentration (c) when the wavelength of the incidence light is fixed. Lambert-Beer s law states that A l C, where is the constant of proportionality, called the absorbtivity UV/Vis spectrophotometer The UV/Vis spectrophotometer is a general purpose analysis instrument which can be used for all types of basic spectrophotometer methods. It spectrophotometer can be classified by single beam spectrophotometer, double beam spectrophotometer, and double wavelength spectrophotometer according to the difference of optical structure. All types of UV/Vis spectrophotometers are constructed with five basic component, they are light source, monochrometer, cell holder, detector and signal processing system.

6 1.2.3 Condition of measure method The choice of measuring wavelength Normally taking the wavelength which has the most absorbance as the measuring wavelength ( max ) to attain the highest analysis sensitivity is called maximum absorbance principle. The absorbance will change very little during the wavelength s change around the max, giving a good precision. we can take the low sensitivity measuring wavelength as the absorption peak wavelength when measuring high concentration compounds, in order to guarantee the corrective curve has enough linear range. If the absorption peak in the wavelength max is too thin, we can adopt a little lower sensitivity wavelength to measure the condition that satisfies the need of analysis sensitivity, which is to decrease the deviation of Beer s Law. The choice of absorbance range Because of the instability of the light source, inaccuracy of the readings, or alternation of lab condition in the measurement, any photometer has some measuring error. Because the transmittance T in the absorbance law is a negative logarithm to the concentration C, from the curve of negative logarithm we can see, the relative error of the same transmittance in a different concentration is different. The relative error is very big when the concentration is too high or too low, so we should choose the correct absorbance range to reduce the relative error of the results. In practice, we can adjust the concentration of the solution or the length of the cell to make sure that the absorbance as in the required range. The choice of bandwidth Bandwidth will affect the sensitivity of the measurement and linear range of correction curve. If the bandwidth is too wide, the monochromatic light of incidence will be less, the correction curve will deviate from Beer s Law, and the sensitivity will be lower. If the bandwidth is too narrow, the gain of the instrument will be very high and the noise will be increased. We should choose the correct bandwidth by looking at the scan of a peak and the amount of absorption for the given standard solution to be analysed.

7 1.3 Components description Figure 1.1 shows the basic T8DS instrument. Figure 1.1 Instrument Front view The front view is shown in Figure 1.2, the name and function of all the components are described below: Figure 1.2 Front view

8 1. Instrument cover 2. Front panel of the sample compartment standard front panel for the sample compartment. It can be replaced when using some accessories. 3. Chassis the steel chassis can greatly reduce vibration. 4. Instrument label 5. Sample compartment cover Open the cover to gain access to the sample compartment Rear view The rear view is shown as Figure 1.3, the name and function of all components are described below: Figure 1.3 Rear view 1. Fan 2 Foot Shockproof rubber washer is used. 3 RS-232 interface Communication with PC. 4 Power supply Connect to power supply: AC 110V, 60Hz. 5 Fuse 1 Can be replaced (refer to Appendix 3 fuse replacement ). 6 Fuse 2 Can be replaced (refer to Appendix 3 fuse replacement ). 7 Instrument nameplate

9 1.3.3 Side view The side view is shown as Figure 1.4, the name and function of all components is described below: A Left side view B Right side view Figure 1.4 Side view 1. Power switch 2. Light source cover Open the cover to gain access to the light source, For replacing the deuterium lamp and tungsten lamp (refer to Appendix 1 light source replacement ) Sample cell holder The sample cell holder is configured according to the user s requirements. The general configuration is the fixed two cell holder. Other types of cell holders are available. Please refer to chapter 4Accessories for detailed information. The following figure 1.5 shows the fixed cell holder which is used as the standard configuration. It has two standard holders which are used for the sample cell and reference cell. Figure 1.5 Fixed cell holders

10 1.4 Specifications Figure 1-3 Item Wavelength range Spectral bandwidth Resolution Setting wavelength Wavelength accuracy Wavelength reproducibility Wavelength of lamp change Photometric system Photometric scope Recording scope Photometric Accuracy Photometric reproducibility Stray light Baseline flatness Stability Noise 900nm 190nm Specification 5nm 2 nm 1 nm 0.5 nm 0.2 nm 0.1nm ( 6 steps) 0.01nm The start and end wavelength can be set by the span of 1nm. The goto-wavelength operation can be set by the span of 0.1nm. ±0.3nm (with built-in automatic correction) 0.1nm Set the wavelength of lamp change within the scope of nm at 1nm interval Double beam, dynamic feedback direct ratio recording system Absorbance: -4 4 Abs Absorbance: Abs Transmittance: %T ±0.002Abs (0 0.5Abs) ±0.004Abs ( Abs) ±0.3%T (0 100%T) 0.001Abs 0 0.5A 0.002Abs 0.5 1A 0.15 % 0.02%T 220nm NaI 10g/L ±0.001 Abs ( scan with 850~200nm, with medium speed, at 2nm spectrum bandwidth ) Abs/h (2hr warm-up, kinetic scan at 500nm with 2nm spectrum bandwidth) Abs (500nm, with 2nm spectrum bandwidth) 0.2 (500nm with 2nm spectrum bandwidth) Note: 1. The above specifications are taken with a 2nm spectrum bandwidth. The specification may vary with different bandwidths 2. The above specifications are subject to change without notice.

11 Chapter 2 Installation 2.1 Installation location T8DS double-beam UV/Vis spectrophotometer is a versatile high-precision laboratory instrument. For its optimum performance and its usable longevity, the instrument should be installed in a suitable location with the following requirements: Avoid high temperature and high humidity environment. An environmental temperature should be 15C 35C. The relative in-door humidity should be 45 85%. The instrument should be placed on a sturdy workbench that is free of a strong vibration. The location room should be free from strong electromagnetic interference and harmful or poisonous gases. Power Supply: 110V±10%, 60Hz±1Hz. A voltage regulator (500VA) should be used if the supply is noisy or irregular. A satisfactory earth connection should be ensured. 2.2 Installation T8DS comprises of three major components: 1. A UV/Vis spectrophotometer main unit. 2. An IBM-compatible Personal Computer complete with monitor and keyboard. The computer can be supplied by user but an RS232 socket should be available. 3. Software: The operating software is UVWin. This should be setup and installed at the computer with attention to the S/N which is supplied with the instrument. For detailed information please refer to the UVWin manual. The connections should be carried out as shown in Figure 2.1:

12 Figure 2.1 Connect the instrument s RS 232 communication port to the PC with RS 232 cable. Connect the printer s parallel port or USB port to the PC with communication cable, and setup the printer driver in the PC (the detailed information refer to the printer manual) Both ends of all the connecting cables should be securely tightned to the sockets to prevent poor connection. Connect the power cords of the instrument, PC, and printer to the power supply connector. (Note: make sure that the rating of the power source is 110VAC 60 HZ.) Note: The spectrophotometer is a precision electronic instrument. Take care not to pull out or insert the power cable when the instrument is switched on, as this could cause serious damage to the instrument or the computer.

13 2.3 Start Make sure there is nothing installed in either of the sample cells which could block the light path. Turn on the power for the printer, then the power for the computer and finally the power for main unit. The computer will start OS automatically. Select UVWin software in the Start menu. The instrument will start to Self Check providing it detects the instrument, (shown as figure 2.2). If the software shows: Warning: Unable to communicate with main unit before the self check, it means that the software cannot communicate with the instrument. Please check the instrument and PC communication connection. Restart the instrument and choose Retry menu. Figure2.2 Initialization Note: If an error occurs during the initialization after power on, please try and restart the instrument. If it still cannot initialize normally, please contact your local distributor or service center. After self checking, enter main working program (shown as figure 2.3). The analysis should be carried out after a preheat time of 60 minutes after switching on the instrument in order to insure the precision of the results. For detailed operation we recommend that you are familiar with the operation of the instrument and the software by referring to this instruction manual, The UVWin software or help document in the software menu. After the analysis is complete, the power can be switched off by first turning off the power supply for main unit, then the power supply for printer, at last the power supply for computer.

14 Figure 2.3 UVWin interface 2.4 Installation performance Performance checks of the instrument should be carried out after installing the instrument. During the course of its life, periodical tests should also be made. The checks should only be carried out after preheating the instrument for at least 60 minutes after switching on. The testing method can be performed as the instructions below. Note: There may be some drifting of the instrument during the preheating, so please carry out wavelength correction and dark current correction prior to analysis in order to obtain the best accuracy. For more detailed instruction please refer to the UVWin software manual The accuracy and reproducibility of wavelength The wavelength accuracy of the instrument is ±0.3nm whereas its reproducibility is 0.1nm (Please refer to the Chapter 1.4 Specification). The test should be made in the following manner by using the two characteristic spectrum lines of the deuterium lamp. Set the parameters by using the spectrum scan function (refer to UVWin software manual) as shown in table 2-1 and table 2-2:

15 Table nm characteristic spectrum Scan parameter Comment Photometric Es Energy for sample light Scan speed Medium Sample interval Automatic 1nm Energy condition D2 lamp, gain 2 /3 Reference Wavelength range nm Vertical coordinate range Instrument parameter Comment Spectrum 2.0nm Fixed or variable Table nm characteristic spectrum Scan parameter Comment Photometric Es Energy of sample light Scan speed Medium Sample interval Automatic 1nm Energy condition D2 lamp, gain 2/3 Reference Wavelength range nm Vertical coordinate range Instrument parameter Comment Spectrum bandwidth 2.0nm Fixed or variable Scan three times and pick the peaks. Note the three peaks and calculate the accuracy of the wavelength. Calculate the mean value of wavelength according to the formula Formula: 1 n n i 1 i measured value of wavelength n measured times, here n=3 i The difference in value between the mean value and the standard value is the wavelength accuracy. The difference in value between the maximum and the minimum is the wavelength reproducibility.

16 2.4.2 Flatness of the baseline Testing method: Check that the sample beam is blank (empty with no solution). Then set the measuring parameters by using the spectrum scan function (refer to the UVWin software manual) as shown in table 2-3 Table 2-3 measure the flatness of baseline Scan parameter Comment Photometric mode Abs Energy of sample light Scan speed Slow Sample interval Automatic 1nm Wavelength range nm Vertical coordinate range Instrument parameter Comment Spectrum bandwidth 2.0nm Fixed or variable Correct the baseline first. Then set the range of wavelength to nm, and select start for spectrum scanning. Read the absorbance of the spectrum scan by the graph reading function. The largest absorbance should conform to the requirement of the flatness of the baseline specification.

17 Chapter 3 Instrument operation All of the operation of T8DS is performed by the UVWin software after connection with the PC. Please read the UVWin software manual in detail before operating. This chapter will introduce the character of double beam measurement, and the process of operation of the T8DS using three examples. 3.1 Double beam measurement What is double beam The T8DS double beam UV/Vis spectrophotometer has two light beams who s energy for the measured sample and reference are the same. This optical principle (as shown in figure 3.1, R means reference light beam and S means sample light beam), increases the stability and precision of the instrument by the use of the real time feedback compensation measuring system of the reference beam. The most differences between double beam, split beam and single beam on structure is that the double beam instrument has two light beams in the sample compartment. Reference and sample can be measured at the same time (as shown in figure 3.2).

18 Figure 3.1 Optical Principle Reference cell holder Sample cell holder Figure 3.2 Sample cell holder How to use a double beam instrument The difference between double beam and single beam (or split beam) for the analysis is, for single beam you should put the blank and sample into the same sample cell holder, measuring twice, for blank and sample. Double beam is read just once for reference and sample. For double beam instruments, put the black block into sample light beam cell holder to do the dark current correction. You can familiarize yourself with the operation of the T8DS by the following examples.

19 3.2 Application examples Photometric measurement example Vitamin B1 can promote the metabolizability of carbohydrate and fat, provide energy for the nervous tissue, prevent the nervous tissue from atrophy and degeneration, prevent and cure beriberi. The quality determination method of Vitamin B1 for the pharmaceutical industry is to measure the absorbance at 400nm; The conforming value should be less than We need to select the photometric measurement function to determine the quality of Vitamin B1 by UVWin software, the detailed operation steps follow: : Prepare reagent Weight 1g Vitamin B1 in a precision microbalance. Put the 1g of Vitamin into a 10ml volumetric flask. Add adequate distilled water to dissolve the Vitamin B1. Select two clean matched quartz cells to fill with distilled water as the reference solution. Power on the instrument Power up the PC which is connect with the T8DS, enter into the Windows operating system. Be sure there is nothing blocking the beam of the sample cell holder, and power on the instrument. Start UVWin software and allow the instrument to initialize. Enter the main working program. The measurement can only be performed after the preheat time of 60 minutes after switching on the instrument.. Setting parameters Select the Photometry function and enter into the parameter setting interface. Set the parameters as follows: Table 3-2 (Photometric measurement example parameter settings) Measurement parameters Instruction Photometric mode Abs Measurement wl 400nm Instrument parameter Instruction Spectral bandwidth 2.0nm Fixed or variable

20 Dark current correction Insert the black block into the sample cell holder, to carry out the dark current correction using the dark current correction function of the UVWin software. Take out the black block after correction. Note Dark current correction can eliminate some noise of the instrument, and insure the precision of result. This does not have to be carried out for every measurement, only when the environment has been changed, such as the temperature, the location, measuring high absorbance sample and so on. (we advise that you perform the dark current correction after preheating and before measurement.) Zero Put the two matched quartz cells which are filled with distilled water into the sample light beam cell holder and reference light beam cell holder. Cover the sample compartment and press the Zero button of the UVWin software. The absorbance shown on the top of the main page should be Abs. Measure the sample Take the cell out of sample cell holder, and replace the distilled water with the Vitamin B1 solution. Be sure to wash out the cells between samples. Put the cell into the sample cell holder and cover the sample compartment. Press the Start button of the UVWin software to perform the measurement. After finishing the measurement, press Start again to measure the next data. The result can be made more accurate by the averaging of several measurements. Analyze the result The result can be saved as a special file format of UVWin software for checking and printing later Spectrum measurement example Vitamin B12 s characteristic absorption peak is at 361nm, so the quality determination method of Vitamin B12 is to measure the absorbance at 361nm. The detailed operation steps of determining the absorption peak of Vitamin B12 by T8DS is as follows: Prepare reagent The Vitamin B12 solution can be mixed with distilled water according to the proportion of 1:10 to obtain a 10ml diluted solution. Prepare two clean matched quartz cells to fill with distilled water as the reference solution.

21 Power on the instrument Power up the PC which is connected with the T8DS and enter into the Windows operating system. Be sure there is nothing in the sample cell holder to block the beam and power on the instrument. Start UVWin software and allow to initialize. Enter the main working program. The measurement can only be performed after the preheating time of 60 minutes after switching on the instrument. Setting parameters Select the Photometric function and enter into the parameter setting interface. Set the parameters as follows: Table 3-2 (Spectrum measurement example parameter settings) Measurement parameters Comments Photometric mode Abs Scanning speed Medium Scanning interval 1nm Wavelength range nm Vertical coordinate range Instrument parameters Comments Spectral bandwidth 2.0nm Fixed or variable Dark current correction Insert the black block into the sample cell holder., Carry out the dark current correction using the dark current correction function of the UVWin software. Take out the black block after correction. Note Dark current correction can eliminate some noise of the instrument, and insure the precision of result. This does not have to be carried out for every measurement, only when the environment has been changed, such as the temperature, the location, measuring high absorbance sample and so on. (we advise that you perform the dark current correction after preheating and before measurement.) Baseline Place the two matched quartz cells which are filled with distilled water into the sample cell holder and reference cell holder. Cover the sample compartment and select the Baseline button of the UVWin software. The result of the baseline will be shown on the graph. Please wait for it to finish automatically, it may take several minutes. During this process no other operation of the software can be performed but it can be stopped by

22 pressing the Cancel button, and the data of correction will be lost. Measure the sample Remove the cell from the sample cell holder and replace the distilled water with the Vitamin B12 solution. Be sure to wash the cells between samples. insert the cell which is filled with sample solution into sample cell holder and cover the sample compartment.press the Start button of the UVWin software to begin the spectrum scanning. After finishing measurement automatically, it will take several minutes, press the Start again to measure the next data. The result can be made more accurate by the averaging of several measurements. During this process no other operation of the software can be performed. if it is necessary to stop the operation please press the Cancel button and the scanning spectrum will be saved. Note: Please pay attention to the position of the cell when taking it out as it needs to be consistent to insure minimum error. Analyze the result You can use the Peak-picking function of software to analyze the spectrum after finishing the measurement. (By the shortcut of Peak-picking or under the Graph menu) You can search for the peak by this peak picking function although it may be necessary to re-set the threshold. The software will list the result of measurements corresponding to the peaks.. Result output You can save the result of the spectrum and the peak-picking as a special file format of UVWin software for checking and printing later Quantitative measurement example [Cr(VI)] detection is an important item for the detection for electronic and electrical products. Take Diphenylcarbazide. The UV/Vis spectrophotometer method can detect the concentration of [Cr(VI)] in electronic and electrical products. The detailed operation of determining the concentration of [Cr(VI)] by T8DS is as follows: Prepare reagent First prepare the following solution. Water used for these solution should be distilled water, and the reagent should be analytical pure. Sulphuric solution (1+9): sampling 10 ml sulphuric GR and mix it into 90mL of water slowly. Nitric acid solution (5 mol/l): sampling 31mL nitric acid (GR) and add it

23 into 69mL water.. Leaching solution: weight 20.0g sodium hydroxide and 30.0g anhydrous sodium carbonate. Dissolve them in distilled water and remove into 10ml volumetric flask. Remove into plastic bottle for preservation. Buffer solution: dissolve 87.09g of dipotassium phosphate and 68.04g potassium dihydrogen phosphate in distilled water, and remove into 1000mL volumetric flask.(ph=7). [Cr(VI)] stock standard solution 100mg/L: measure g potassium dichromate exactly and dry under 120C for 2 hours. Dissolve it with distilled water and remove into 1000 ml volumetric flask. [Cr( )] standard solution 5.0 mg/l: measure 5.0ml stock standard solution into 100 ml volumetric flask. Dissolved it in distilled water and mix. Diphenylcarbazide (DPC) chromogenic agent: weight 0.5g DPC into 100 ml acetone, preserve in brown bottle. If the solution s color fades, re-prepare it. Dispose the sample Disposal of the electronic and electrical products have been split into strips or powder samples which have a diameter of no more than 1 mm and a length of no more than 5 mm by a crusher. Weight (0.5~2.5)g precision to 1mg sample exactly into a conical flask and add into the 25.0 ml leaching solution. Add also to the 0.5 ml buffer solution. The sample should be submerged in the leaching solution, and mixed round in a(90~95)c water bath (or shaking bath ) for 1.5 hours. Remove the sample and cool it down to room temperature. Filtrate and wash the conical flask with water Collect the filtrate and cleaning solution into a beaker and add 5 mol/l nitric acid into it, Control the ph value of solution in the range of 7 to 8 measuring with a ph meter. Filtrate further if required, keeping the filtrate. Power on the instrument Power up the PC which is connected with the T8DS and enter into the Windows operating system. Make sure there is nothing blocking the sample beam and power on the instrument. Start UVWin software and the instrument will carry out the initialization. Enter the main working program. The measurement should only be performed after an interval of preheating lasting 60 minutes after switching on the instrument.

24 Setting parameters Select the Quantitative function and enter into the parameter setting interface. Set the parameters as follows: Table 3-2 Quantitative measurement parameter settings Measure method Main WL Calibration curve Equation Order Conc. Unit Calibration method Measurement parameters Single wavelength 540nm Abs=f(c) 1 st mg/l Concentration method Instrument parameters Comments Comments Spectral bandwidth 2.0nm Fixed or variable Color producing reaction Standard solution: sampling 0.0, 2.0, 4.0, 6.0, 8.0, 10.0, 12.0mL [Cr(VI)] standard solution (5.0 mg/l) and pipette it into 100mL volumetric flask. Add 50mL water into it, and add 2.0mL Diphenylcarbazide color producing reagent. Mix. Drop 2 beads of vitriol solution (1+9) and make the ph value of the filtrate in the range of 1.5 to 2.5, make up to volume with water. The concentrations of [Cr( )] in these calibration solution are 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6mg/L. Mix, shake and leave to settle for half an hour. Sample solution: Add 2.0mL Diphenylcarbazide color producing reagent into sample filtrate. Mix and add drop vitriol solution (1+9). Make the ph value of filtrate in the range of 1.5 to 2.5, and move all the filtrate into a 100mL volumetric flask. Make up volume with water. Mix, shake and leave to settle for half an hour. Establish the calibration curve Input the ID and concentration of the standard solutions from 1 to 7 in the Standard table. The concentrations are 0.0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6 mg/l. Put the two matched quartz cells which are filled with blank reagent solution into the sample cell holder and reference cell holder. Cover the sample compartment and press the Zero button of the UVWin software. The absorbance shown on the top of the main screen should be Abs or. Replace the solution in the sample cell with the [Cr(VI)] standard solutions from NO.1 to NO.7 and press Start to measure the absorbance. The software will plot the calibration curve between Concentration and Abs in real time (as shown below).

25 Table 3.3 Calibration Curve The parameters of calibration curve are: Abs = K1*(C) + K0 K0= K1= R2= Measure the sample Input the ID of the sample in the Sample table using the same conditions and measure the Abs of sample solution and blank solution. The software will calculate the concentration of [Cr(VI)] by using the calibration curve, expressed as A and B. Analyze the result After the measurement, calculate the mass fraction W, units shown as mg/kg. The concentration of [Cr(VI)] is mg/kg by the formula below: ( A B) * V * N W m W - Concentration of [Cr(VI)] in the sample, the unit is mg/kg A - Concentration of the leaching solution from the calibration curve. The unit is mg/l. B - Concentration of the blank solution from the calibration curve. The unit is mg/l V - Constant volume of leaching solution The unit is ml N - Dilution multiple of leaching solution. M - Mass of sample, the unit is gram (g)

26 Chapter 4 Optional accessories 4.1 CH19-1 Thermostatic cell holder The thermostatic cell holder is used together with a constant-temperature water bath and water pump. It is designed to measure samples at a constant and accurate temperature. The picture and specification are shown below. Figure 4.1 Thermostatic cell holder Table 4.1 specifications NO. Item Specifications Remark 1 Product model CH Connection tube Inner diameter 4mm 3 Wavelength range nm 4 Path length 10mm 5 Cell holder NO. 2 Sample beam and reference beam sample holder

27 DS19-1 Angle-changeable solid sample holder Sliced solid samples can be installed onto the angle-changeable solid sample holder. The angles can be adjusted within ±45 and it is easy to measure the absorbency for solid samples.. The picture and specification are shown below. Figure 4.2 Angle-changeable solid sample holder Table 4.2 Specifications NO. Item Specifications Remark 1 Product model DS Wavelength range nm 3 Changeable angle range ±45o 4 Min. sample size 4mm 5 Max. sample size 80x55x5mm

28 IS19-1 Integrating sphere The integrating sphere is used to measure the diffuse reflectance of solid sample and powder, as well as measure the transmittance of glass and membrane. The integrating sphere can analyze the chrominance, color difference and whiteness. The picture and specification are shown below. Figure 4.3 Integrating sphere Table 4.3 Specifications NO. Item Specifications Remark 1 Product model IS Incident angle Sample light beam 0 Reference light beam8 3 Min. sample dimensions Width 15mm Height25mm Diffuse reflectance 4 Min. sample dimensions Diameter 20mm Transmittance 5 Wavelength range 230nm-850nm Slit 5nm 6 Sphere diameter 60mm

29 LS19-1 Long pathlength cell holder The long pathlength cell holder can be used with 5-50mm wide cells making it is easy for the measurement of samples. The picture and specification are shown below. Figure 4.4 Long pathlength cell holder Table 4.4 Specifications NO. Item Specifications Remark 1 Product model LS Wavelength range nm 3 Pathlength 5mm 10 mm 20mm,30 mm 40 mm 50 mm Adjusted according to requirements 4 Cell NO. 2 Sample light beam and reference light beam

30 MH19-1 Micro cell holder Micro cuvettes can be used in the micro cell holder. The bases can be carefully adjusted to enable the light path to pass through the cell windows giving maximum light throughput and improve measurement precision for micro samples. The picture and specification are shown below. Figure 4.5 Micro cell holder Table 4.5 Specifications NO. Item Specifications Remark 1 Product model MH Wavelength range nm 3 Cell NO. 2

31 MH19-2 Ultra-micro cell holder Ultra-micro cuvettes need to be used with the ultra-micro cell holder due to the clear aperture on the cuvettes being very small. Using a standard cell holder for the measurement would block some light causing the energy to be lost and the instrument precision reduced. Two quartz lens are used to shrink the imaging of the beam in the sample and reference optical circuits through the ultra-micro cell holders. After this the beams are magnified by two more quartz lenses which collect energy and return back to normal state to be read by the detector. By using this accessory the signal-noise ratio and measurement precision of the instrument will be greatly improved. The picture is as figure 4.6 shown; the specification is as Table 4.6 shown. Figure 4.6 Ultra-micro cell holder Table 4.6 Specifications NO. Item Specifications Remark 1 Product model MH Wavelength range nm 3 Cell NO. 2

32 MR19 1 Specula reflection accessory The specula reflection accessory can measure the reflectance spectrum of optical surfaces, crystals and coated samples. If the reflecting mirror on the reference beam is the standard reflecting mirror, the user can calculate the absolute reflectivity of the measured surface. The picture and specification are shown below. Figure 4.7 Specula reflection accessory Table 4.7 Specifications NO. Item Specifications Remark 1 Product model MR Incidence angle 5o Measured sample 11 9mm to 60 40mm 3 area 4 Wavelength range 190nm-900nm

33 MS19-1 Manual 8-cell holder Manual 8-cell holder is ideal for multi-sample measurements. Up to 8 samples can be put in the cell holder for separate measurement. The picture and specification are shown below. Figure 4.8 Manual 8-cell holder Table 4.8 Specifications NO. Item Specifications Remark 1 Product model MS Wavelength range nm 3 Cell NO. 9 Reference cell holder:1 Sample cell holder:8

34 PS19-2 Sipper pump The sipper pump accessory consists of a sipper pump, front baffle and connection tubes. The sipper pump is a soft-tube pump that can transmit liquid in dual directions. It is widely used in research and production for refine chemistry, biophysics, biochemistry, environmental protection, pharmaceuticals and other industries. It is an ideal device for transmitting sticky and corrosive liquids. The PS181-2 sipper pump accessory has the following features: 1. LCD displays liquid sampling or motor rotation speed. All functions and parameters can be set from six buttons. 2. It can store data if the power supply is lost. The device can automatically store the sampling volume or the rotation speed of the motor. The LCD displays the value that is set in the last operation when it is turned on. 3. It has a new control system and quantitative sampling system. There are two working modes, continual and quantitative. It can be used for continuous sampling and discontinuous quantitative sampling. 4. It has an auto-calibration function. Users can calibrate the sampling volume through the calibration function which will avoid errors with prolonged running. 5. The mixing steper-motor runs smoothly and accurately with large torque and low noise through a high-subdivision driver. 6. The membrane touch-switches are easy to operate and the tube clips are easy to install and dismantle. 7. It is easy for maintenance. For different fluids it is only necessary to replace the soft tube. There is no pollution from the valves or sealing parts. 8. It can transmit liquids from dual-direction, have accurate quantitative sampling, have stable flow rate and be used with an outside interface control. The picture and specification are shown below.

35 Figure 4.9 Sipper Pump Table 4.9 Specifications NO. Item Specifications Remark 1 Product model PS Rotation speed range rpm Clockwise & counterclockwise 3 Speed resolution 0.1rpm: lower than 30rpm 1 rpm: higher than30rpm 4 Display mode 3 1/2 LCD display 5 Sampling accuracy 1 ml 6 Power supply AC85v-264v, 50-60Hz 7 Working environment Temp: 0-400C, Relativity humidity<80% 8 Driver size (L*W*H)370*210*500(mm) 9 Driver weight 10kg

36 S19-1 Solid sample holder Sliced solid samples can be put in the solid sample holder which makes it easy to measure the absorbency. The picture and specification are shown below. Figure 4.10 Solid sample holder Table 4.10 Specifications NO. Item Specifications Remark 1 Product model S Wavelength range nm 3 Cell NO. 2 4 Max. sample size 80x55x5mm

37 SS19-1 Short pathlength cell holder The short pathlength cell holder is inserted into the standard cell holder making is easy to measure samples using short pathlength cells. The short pathlength cell holder can be used in the following holders: standard fixed cell holder, 8-cell holder, micro cell holder and ultra-micro cell holder. The picture and specification are shown below. Figure 4.11 Short pathlength cell holder Table 4.11 Specifications NO. Item Specifications Remark 1 Product model SS Wavelength range nm 3 Path length 1mm 2mm 5mm

38 TR19-1 Test tube cell holder The test tube holder is used for the measurement of liquids contained in test tubes. The measurement results are dependent on the material and quality of the test tubes. Therefore if precise measurement is required, it is recommended that the related accessory for cuvettes be used. The picture and specification are shown below. Figure 4.12 Test tube cell holder Table 4.12 Specifications NO. Item Specifications Remark 1 Product model TR Wavelength range nm 3 Test tube range Diameter: 15 25mm Height: mm 4 Cell NO. 2

39 Chapter 5 Maintenance The T8DS UV-VIS Spectrophotometer is a precision instrument. Careful assembling and final test have been carried out before delivery. Appropriate routine attention and maintenance will not only ensure the reliability and stability of the instrument but also extend its operating lifetime. 5.1 Points for attention: a. A good environmental condition should be provided according to the requirements in Section 2.1 Site requirement b. Since the instrument has been adjusted to its optimum conditions before delivery, users are requested not to adjust it by themselves nor dismount any parts from the instrument, paying special attention not to touch and damage the surfaces of optics Daily care c. Check if there is any spilt sample solution contained in the sample compartment after each measurement. The sample compartment should be cleaned frequently to avoid corrosion to the parts and optical the system. d. The instrument should be covered with an anti-dust cover, which is provided. Silica-gel bags can be put in the sample compartment and the light source housing to keep dry, but be sure to take the bags out before switching on the instrument. e. Periodically check the performance of the instrument and If anything abnormal occurs, contact your local agent or the manufacturer immediately. f. If the instrument is not to be used for a long time, pay great attention to environmental conditions such as temperature and humidity and periodically replace the silica-gel bags. It is recommended to turn on the instrument once a month.

40 5.3 Trouble shooting and maintenance The instrument begins to initialize after turning on and connecting with the PC. The system gives status information after each operation has been completed. If no abnormality is detected, it displays OK. If an abnormality is detected, it displays Err and asks whether the initialization should continue or not. The user can check the status of instrument according to figure 5.1.

41 Table 5.1 Trouble shooting Phenomena Causes Diagnoses Remedy A. Power cable is not A. Check the power A. Connect it securely The instrument does not securely connected cable operate at all, after the B. Fuse is blown B. Check the fuse B. Replace the fuse (2A) power is turned on. C. Check the C. Circuit failure C. Contact our service personnel instrument A. Printer failure A. Check printer A-B. Contact our service personnel Spectrum cannot be B. No driver for printer B. Install the driver printed out. Initialization abnormality: Filter origin W lamp energy D2 lamp energy Wavelength check Noise abnormality C. The connection cable loosen A. Filter mechanism failure Opaque object in the sample compartment A. W lamp is not lit A. Opaque object in the sample compartment D2 lamp is not lit A. Opaque object in the sample compartment B. Wrong positioning of D2 lamp C.WL mechanism failure there is noise A. Light source ageing B. Wrong position of the sample compartment C. Low voltage / strong magnetic field D. Receiver ageing E. Preamplifier board failure F. Abnormality of AD converter C. Check the connection cable A. Switch on power again to check A. Switch on power again to check B. Open the sample compartment B. Open the light source housing A. Open the sample compartment B. Open the light source housing C. Remove the cover of instrument A. Open the sample compartment B. Open the light source housing C. Open the base A. Measure in Energy mode B. Observe at 550nm C. Check voltage/source of magnetic field D. Measure in Energy mode E. Check the preamplifier board F. Check the drive board C. Connect the connection cable securely A. Contact our service personnel A. Contact our service personnel B. Remove the opaque object B. Replace the W lamp A. Remove the opaque object B. Replace the D2 lamp C. Replace the fuse of D2 lamp 0.5A A. Remove the opaque object B. Check the position of D2 lamp C. check the following document A. Replace the light source B. Reposition the sample compartment C. Add voltage stabilizer /eliminate interference D-F. Contact our service personnel

42 Note: If the initialization is abnormal, please confirm as the following steps first and then operate according to the upper table. Check the cable that connects the main unit with the PC. Power off (or quit the OS), initialize again, and check if the same error still appears. Reinstall UVWin software and initialization again; check if the same error still appears. About the disposal of wavelength mechanism failure On some accidental conditions such as illegal operation, the nut will overstep its range and become locked causing the drive motor to be noisey as it can t rotate the nut. If you hear a noise when initializing Wavelength checking. you can fix the problem according to the following steps: Put the instrument on its side as figure 5.1, rotate the screws on the base and remove panel. Find the scanning mechanism as figure 5.2, check the mechanism of the instrument according to the picture. Check which end the nut stops. If the nut stops as the picture shown, rotate the connecter counterclockwise, making the nut move freely on the guide screw. If the nut stops at the other end, rotate the connecter clockwise. Note: Do not touch the guide screw with your hand or any other object in case of damage to the guide screw which will affect the precision of the wavelength mechanism. Figure 5.1 Instrument position

43 Figure 5.2 Wavelength mechanism

44 Appendix 1 Light source replacement Replace the tungsten lamp The tungsten lamp is plugged in to a socket and sleeved by a plastic holder. It is well adjusted before delivery. If you need to replace the tungsten lamp, please observe the following procedures to replace it. Figure 6.1 Tungsten lamp set Open the light source cover. Disassemble the two fixing screws of the light source cover, and remove as figure 6.2. Figure 6.2 Open the light source house cover Loosen the two fixing screws on the tungsten lamp socket and remove the tungsten lamp set, as shown in figure 6.3

45 Figure 6.3 Loose screws Replace with a new tungsten lamp. Clean the surface of the tungsten lamp with a clean cloth soaked in alcohol. Insert the tungsten lamp holder into the tungsten lamp socket in the light source housing and tighten the two holding screws. Pay attention to the direction of the filament. Replace the light source cover. Figure 6.4 Filament direction If the performance of the instrument changes greatly after the replacement, the height of tungsten lamp should be adjusted (The horizontal position of tungsten lamp is adjusted automatically when the self-testing is done upon switching on the power.). First, remove the tungsten lamp holder, loosen the adjusting screw on the tungsten lamp holder and adjust the height of tungsten lamp. (As figure 6.1) The distance between the center of the filament and the bottom should be 40mm according to the design requirements, but it can be adjusted slightly. Tighten the setscrews and insert the W lamp holder back in to the socket.

46 Replace the Deuterium lamp The D2 lamp is plugged in the D2 lamp socket. When replacement is required, insert a new one into the socket. The procedures is shown as follows: Open the light source cover. Remove the deuterium lamp by pulling it upwards. It may be installed tightly. Figure 6.5 Remove the D2 lamp Clean the surface of D2 lamp with a clean cloth soaked in alcohol. Insert the new D2 lamp into the socket. The key part of the deuterium lamp and the hole of the holder should be aligned (the light beam window should face to the convergent lens), as shown in figure 6.6. Figure 6.6 Insert the D2 lamp

47 Note: 1 The light source and light source housing can become heated during operation, therefore, be sure to turn off the power switch and allow to cool down sufficiently touching. 2 The convergent lens should be covered to avoid being contaminated by fingers or objects while work is carried out..

48 Appendix 2 Fuse replacement This chapter introduces the user how to replace the fuse. If you suspect the fuse is blown, please replace it according to the following procedures. Switch off the instrument. Remove the fuse holder using a plain screwdriver, as shown in figure 6.1 Figure 6.1 Removing the fuse Remove the old fuse, and replace it with a new one. Install the fuse holder back into the instrument. Figure 6.2 Replacing the fuse Note: The instrument takes two kinds of fuse, 2A and 0.5., In case of damage to instrument, please select the same fuse as the old one when replacing it.

49 Persee Analytics Inc. Address:7270 Popham Place, Solon, OH44139, United States Contact:Sean Cao Title:Sales and Marketing Director Tel:(440) Web: