PRODUCTION OF CERTIFIED REFERENCE MATERIAL OF HOLMIUM(III) OXIDE IN AMPOULES

Gonçalves, Debora E. F.; Alvarenga, Ana P. D.; Borges, Paulo P.; Gomes, Juliana F. S.; Araujo, Thiago O.

doi:10.21577/0100-4042.20170292

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Artigo • Quím. Nova 41 (10) • Dec 2018 • https://doi.org/10.21577/0100-4042.20170292 copy

PRODUCTION OF CERTIFIED REFERENCE MATERIAL OF HOLMIUM(III) OXIDE IN AMPOULES

Authorship SCIMAGO INSTITUTIONS RANKINGS

This work reports the development of a certified reference material (CRM) of holmium(III) oxide Ho₂O₃ in acidic solution for the wavelength scale calibration of UV-Vis spectrophotometers. A 4.0% Ho₂O₃ solution was gravimetrically prepared in 10% perchloric acid and bottled in 5.0 mL glass ampoules. Homogeneity, stability and characterization were assessed according to ISO 17034 and ISO Guide 35. The material certification was undertaken by two laboratories by using UV-Vis spectrophotometry for characterization of the 14 peaks of minimum transmittance of Ho₂O₃, using a spectral bandwidth of 1.00 nm and a scanning speed of 30.0 nm min^‒1. The material property values in wavelength (nm) were obtained for these 14 peaks, together with the expanded uncertainty (U) of 0.12 nm, for a coverage factor (k = 2.00) corresponding to a probability of approximately 95%, which took into account the standard uncertainties obtained in each study performed for the certification of the produced reference material.

Keywords:
holmium(III) oxide; certified reference material; spectrophotometry; wavelength; calibration

Valor nominal do pico (nm)	F _calculado	p-valor
241	1,87	0,08
249	1,93	0,07
278	1,62	0,13
287	0,81	0,61
333	0,75	0,66
345	0,96	0,48
361	0,65	0,75
385	0,91	0,52
416	1,89	0,08
451	1,37	0,23
467	1,40	0,21
485	1,11	0,38
536	0,27	0,98
640	0,93	0,51

Valor nominal do pico (nm)	4 ºC		25 ºC		50 ºC
Valor nominal do pico (nm)	\|β₁\|×10^‒5	(sβ₁ t_st)×10^‒5	\|β₁\|×10^‒5	(sβ1 t_st)×10^‒5	\|β₁\|×10^‒5	(sβ₁ t_st)×10^‒5
241	18	34	12	30	29	38
249	11	74	2	59	5	83
278	47^a a Valores de \|β1\| maiores que sβ1tst.	37	8	29	61^a a Valores de \|β1\| maiores que sβ1tst.	37
287	33^a a Valores de \|β1\| maiores que sβ1tst.	32	28	30	29	37
333	33	64	6	67	40	63
345	51	102	80	112	39	108
361	16	37	43^a a Valores de \|β1\| maiores que sβ1tst.	36	24	51
385	22	75	22	67	42	66
416	54^a a Valores de \|β1\| maiores que sβ1tst.	44	47^a a Valores de \|β1\| maiores que sβ1tst.	45	69^a a Valores de \|β1\| maiores que sβ1tst.	38
451	23	99	7	105	3	116
467	3	27	13	31	14	28
485	9	31	27	33	26	33
536	46^a a Valores de \|β1\| maiores que sβ1tst.	42	3	33	8	37
640	22	61	8	45	7	50

Valor nominal do pico (nm)	\|β₁\|×10^‒6	(sβ₁ t_st)×10^‒6
241	35	47
249	32	82
278	16	53
287	22	68
333	2	92
345	8	119
361	38	54
385	77	88
416	23	64
451	25	150
467	2	50
485	4	55
536	40	43
640	4	64

Valores obtidos pelo Laraf	Valores obtidos pela Visomes	Média ponderada
241,25	241,14	241,192
250,00	249,90	249,947
278,22	278,12	278,167
287,33	287,23	287,277
333,57	333,48	333,526
345,47	345,40	345,439
361,33	361,25	361,289
385,71	385,63	385,667
416,35	416,26	416,304
451,42	451,40	451,411
467,88	467,82	467,848
485,30	485,22	485,256
536,62	536,55	536,582
640,55	640,49	640,517

Valor nominal do pico	u _hom	u _ec	u _el	u _car	U _MRC
241	0,004	0,006	0,008	0,044	0,09
249	0,008	0,014	0,015	0,044	0,10
278	0,003	0,021	0,010	0,044	0,10
287	0,002	0,012	0,012	0,044	0,10
333	0,004	0,011	0,017	0,047	0,10
345	0,006	0,019	0,022	0,048	0,11
361	0,002	0,015	0,010	0,045	0,10
385	0,004	0,013	0,016	0,044	0,10
416	0,006	0,024	0,012	0,046	0,11
451	0,009	0,020	0,027	0,048	0,12
467	0,003	0,005	0,009	0,044	0,09
485	0,001	0,006	0,010	0,044	0,09
536	0,003	0,016	0,008	0,044	0,10
640	0,003	0,010	0,012	0,044	0,09

Valor de Propriedade	U
241,19	0,12
249,95	0,12
278,17	0,12
287,28	0,12
333,53	0,12
345,44	0,12
361,29	0,12
385,67	0,12
416,30	0,12
451,41	0,12
467,85	0,12
485,26	0,12
536,58	0,12
640,52	0,12

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Valor nominal do pico (nm)	\|β₁\|×10^‒6	(sβ₁ t_st)×10^‒6
241	35	47
249	32	82
278	16	53
287	22	68
333	2	92
345	8	119
361	38	54
385	77	88
416	23	64
451	25	150
467	2	50
485	4	55
536	40	43
640	4	64

Valor nominal do pico (nm)	\|β₁\|×10^‒6	(sβ₁ t_st)×10^‒6
241	35	47
249	32	82
278	16	53
287	22	68
333	2	92
345	8	119
361	38	54
385	77	88
416	23	64
451	25	150
467	2	50
485	4	55
536	40	43
640	4	64

Valor nominal do pico (nm)	\|β₁\|×10^‒6	(sβ₁ t_st)×10^‒6
241	35	47
249	32	82
278	16	53
287	22	68
333	2	92
345	8	119
361	38	54
385	77	88
416	23	64
451	25	150
467	2	50
485	4	55
536	40	43
640	4	64